Designation: D6866 − 12

Standard Test Methods for

Determining the Biobased Content of Solid, Liquid, and
Gaseous Samples Using Radiocarbon Analysis1
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. 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* information regarding the practice of the art of isotope analysis

1.1 These test methods do not address environmental and to facilitate performance of these test methods.
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
1.2 These test methods are applicable to any product con- require definition of other terms to make sense.
taining carbon-based components that can be combusted in the 3.3 Definitions:
presence of oxygen to produce carbon dioxide (CO2) gas. The 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).
waste incinerators. There are 2.2 by 106 dpm / uCi (14,17).3
1.3 These test methods make no attempt to teach the basic 3.3.2 dps—disintegrations per second (rather than minute as
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
activity per mass unit of product, that is, dpm per gram (14,17).
equivalent to the test methods outlined in this standard.
1.5 This standard does not purport to address all of the 3.3.5 automated effıciency control (AEC)—a method used
safety concerns, if any, associated with its use. It is the by scintillation counters to compensate for the effect of
responsibility of the user of this standard to establish appro- quenching on the sample spectrum (14).
priate safety and health practices and determine the applica- 3.3.6 AMS facility—a facility performing Accelerator Mass
bility of regulatory limitations prior to use. Spectrometry.
2. Referenced Documents 3.3.7 accelerator mass spectrometry (AMS)—an ultra-
sensitive technique that can be used for measuring naturally
2.1 ASTM Standards:2 occurring radio nuclides, in which sample atoms are ionized,
D883 Terminology Relating to Plastics accelerated to high energies, separated on basis of momentum,
3. Terminology charge, and mass, and individually counted in Faraday collec-
3.1 The definitions of terms used in these test methods are tors. This high energy separation is extremely effective in
referenced in order that the practitioner may require further filtering out isobaric interferences, such that AMS may be used
to measure accurately the 14C/12C abundance to a level of 1 in
1
These test methods are under the jurisdiction of ASTM Committee D20 on
1015. At these levels, uncertainties are based on counting
Plastics and are the direct responsibility of Subcommittee D20.96 on Environmen- statistics through the Poisson distribution (8,9).
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
approved in 2004. Last previous edition approved in 2011 as D6866 - 11. DOI: environment; including cosmic radiation and radionuclides
10.1520/D6866-12.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The boldface numbers in parentheses refer to the list of references at the end of
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, PA 19428-2959. United States

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 D6866 − 12
present in the local environment, for example, materials of 3.3.18 effıciency—the ratio of measured observations or
construction, metals, glass, concrete (2,4,7,8,14-19). counts compared to the number of decay events which oc-
curred during the measurement time; expressed as a percentage
3.3.9 biobased content—the amount of biobased carbon in
(14,17).
the material or product as a percent of the weight (mass) of the
total organic carbon in the product (1). 3.3.19 external standard—a radioactive source placed adja-
cent to the liquid sample in to produce scintillations in the
3.3.10 coincidence circuit—a portion of the electronic sample for the purpose of monitoring the sample’s level of
analysis system of a Liquid Scintillation Counter which acts to quenching (14,17).
reject pulses which are not received from the two Photomul- 3.3.20 figure of merit—a term applied to a numerical value
tiplier Tubes (that count the photons) within a given period of used to characterize the performance of a system. In liquid
time and are necessary to rule out background interference and scintillation counting, specific formulas have been derived for
required for any LSC used in these test methods (7,14,17). quantitatively comparing certain aspects of instrument and
3.3.11 coincidence threshold—the minimum decay energy cocktail performance and the term is frequently used to
required for a Liquid Scintillation Counter to detect a radioac- compare efficiency and background measures (14,17,20).
tive event. The ability to set that threshold is a requirement of 3.3.21 fluorescence—the emission of light resulting from
any LSC used in these test methods (14,17). the absorption of incident radiation and persisting only as long
as the stimulation radiation is continued (14,17,25).
3.3.12 contemporary carbon—a direct indication of the
relative contributions of fossil carbon and “living” biospheric 3.3.22 fossil carbon—carbon that contains essentially no
carbon can be expressed as the fraction (or percentage) of radiocarbon because its age is very much greater than the 5730
contemporary carbon, symbol fC. This is derived from fM year half-life of 14C (8,9).
through the use of the observed input function for atmo- 3.3.23 half-life—the time in which one half the atoms of a
spheric 14C over recent decades, representing the combined particular radioactive substance disintegrate to another nuclear
effects of fossil dilution of 14C (minor) and nuclear testing form. The half-life of 14C is 5730 years (8,14,25).
enhancement (major). The relation between fC and fM is 3.3.24 intensity—the amount of energy, the number of
necessarily a function of time. By 1985, when the particulate photons, or the numbers of particles of any radiation incident
sampling discussed in the cited reference the fM ratio had upon a unit area per unit time (14,17).
decreased to ca. 1.2 (8,9). 3.3.25 internal standard—a known amount of radioactivity
3.3.13 chemical quenching—a reduction in the scintillation which is added to a sample in order to determine the counting
intensity (a significant interference with these test methods) efficiency of that sample. The radionuclide used must be the
seen by the Photomultiplier Tubes (PMT, pmt) due to the same as that in the sample to be measured, the cocktail should
materials present in the scintillation solution that interfere with be the same as the sample, and the Internal Standard must be
the processes leading to the production of light. The result is of certified activity (14,17).
fewer photons counted and a lower efficiency (4,7,17). 3.3.26 modern carbon—explicitly, 0.95 times the specific
activity of SRM 4990b (the original oxalic acid radiocarbon
3.3.14 chi-square test—a statistical tool used in radioactive
standard), normalized to d13C = −19 % (Currie, et al., 1989).
counting in order to compare the observed variations in repeat
Functionally, the fraction of modern carbon equals 0.95 times
counts of a radioactive sample with the variation predicted by
the concentration of 14C contemporaneous with 1950 wood
statistical theory. This determines whether two different distri- (that is, pre-atmospheric nuclear testing). To correct for the
butions of photon measurements originate from the same post 1950 bomb 14C injection into the atmosphere (9), the
photonic events. LSC instruments used in this measurement fraction of modern carbon is multiplied by 0.95 (as of the year
should include this capability (14,17,27). 2010).
3.3.15 cocktail—the solution in which samples are placed 3.3.27 noise pulse—a spurious signal arising from the elec-
for measurement in a LSC. Solvents and Scintillators (chemi- tronics and electrical supply of the instrument (14,17,21,29).
cals that absorbs decay energy transferred from the solvent and 3.3.28 phase contact—the degree of contact between two
emits light (photons) proportional in intensity to the deposited phases of heterogeneous samples. In liquid scintillation
energy) (4,7,14,17). counting, better phase contact usually means higher counting
3.3.16 decay (radioactive)—the spontaneous transformation efficiency (14,17).
of one nuclide into a different nuclide or into a different energy 3.3.29 photomultiplier tube (PMT, pmt)—the device in the
state of the same nuclide. The process results in a decrease, LSC that counts the photons of light simultaneously at two
with time, of the number of original radioactive atoms in a separate detectors (29,32).
sample, according to the half-life of the radionuclide (8,14,17). 3.3.30 pulse—the electrical signal resulting when photons
3.3.17 discriminator—an electronic circuit which distin- are detected by the Photomultiplier tubes (14,17,18,32).
guishes signal pulses according to their pulse height or energy; 3.3.31 pulse height analyzer (PHA)—an electronic circuit
used to exclude extraneous radiation, background radiation, which sorts and records pulses according to height or voltage
and extraneous noise from the desired signal (14,17,18,32). (14,17,18,32).

2
 D6866 − 12
3.3.32 pulse index—the number of afterpulses following a cal studies identify a total uncertainty up to 63 % (absolute)
detected coincidence pulse (used in three dimensional or pulse inclusive of indeterminant sources of error in the final biobased
height discrimination) to compensate for the background of a content result. Sample preparation methods include the pro-
liquid scintillation counter performing (14,18,29,32). duction of CO2 within a vacuum manifold system where it is
3.3.33 quenching—any material that interferes with the ultimately distilled, quantified in a calibrated volume, trans-
accurate conversion of decay energy to photons captured by the ferred to a quartz tube, and torch sealed. Details are given in
PMT of the LSC (2,4,7,14,15,17,20). 8.7-8.10. The stored CO2 is then delivered to an AMS facility
for final processing and analysis.
3.3.34 region—regions of interest, also called window
and/or channel in regard to liquid scintillation counters. Refers 4.3 Method C uses LSC techniques to quantify the biobased
to an energy level or subset specific to a particular isotope content of a product using sample carbon that has been
(4,14,18,21,29). converted to benzene. This test method determines the
3.3.35 scintillation reagent—chemicals that absorbs decay biobased content of a sample with a maximum total error of
energy transferred from the solvent and emits light (photons) 63 % (absolute), as does Method B.
proportional in intensity to the decay energy (4,14,29). 4.4 The test methods described here directly discriminate
3.3.36 solvent—in scintillation reagent, chemical(s) which between product carbon resulting from contemporary carbon
act as both a vehicle for dissolving the sample and scintillator input and that derived from fossil-based input. A measurement
and the location of the initial kinetic energy transfer from the of a product’s 14C/12C content is determined relative to the
decay products to the scintillator; that is, into excitation energy modern carbon-based oxalic acid radiocarbon Standard Refer-
that can be converted by the scintillator into photons (4.14,17, ence Material (SRM) 4990c, (referred to as HOxII). It is
29). compositionally related directly to the original oxalic acid
radiocarbon standard SRM 4990b (referred to as HOxI), and is
3.3.37 standard count conditions (STDCT)—LSC condi- denoted in terms of fM, that is, the sample’s fraction of modern
tions under which reference standards and samples are carbon. (See Terminology, Section 3.)
counted.
4.5 Reference standards, available to all laboratories prac-
3.3.38 three dimensional spectrum analysis—the analysis of
ticing these test methods, must be used properly in order that
the pulse energy distribution in function of energy, counts per
traceability to the primary carbon isotope standards are
energy, and pulse index. It allows for auto-optimization of a
established, and that stated uncertainties are valid. The primary
liquid scintillation analyzer allowing maximum performance.
standards are SRM 4990c (oxalic acid) for 14C and RM 8544
Although different Manufacturers of LSC instruments call
(NBS 19 calcite) for 13C. These materials are available for
Three Dimensional Analysis by different names, the actual
distribution in North America from The National Institute of
function is a necessary part of these test methods (14,17,18).
Standards and Technology (NIST), and outside North America
3.3.39 true beta event—an actual count which represents from the International Atomic Energy Agency (IAEA), Vienna,
atomic decay rather than spurious interference (10,11). Austria.
3.3.40 flexible tube cracker—the apparatus in which the 4.6 Acceptable SI unit deviations (tolerance) for the practice
sample tube (Break Seal Tube) is placed (5,6,10,11). of these test methods is 65 % from the stated instructions
3.3.41 break seal tube—the sample tube within which the unless otherwise noted.
sample, copper oxide, and silver wire is placed.
5. Safety
4. Significance and Use 5.1 The specific safety and regulatory requirements associ-
4.1 Presidential (Executive) Orders 13101, 13123, 13134, ated with radioactivity, sample preparation, and instrument
Public Laws (106-224), AG ACT 2003 and other Legislative operation are not addressed in these test methods. It is the
Actions all require Federal Agencies to develop procedures to responsibility of the user of these test methods to establish
identify, encourage and produce products derived from appropriate safety and health practices. It is also incumbent on
biobased, renewable, sustainable and low environmental im- the user to conform to all the Federal and State regulatory
pact resources so as to promote the Market Development requirements, especially those that relate to the use of open
Infrastructure necessary to induce greater use of such resources radioactive source, in the performance of these test methods.
in commercial, non food, products. Section 1501 of the Energy Although 14C is one of the safest isotopes to work with, State
Policy Act of 2005 (Public Law 109–58) and EPA 40 CFR Part and Federal regulations must be followed in the performance of
80 (Regulation of Fuels and Fuel Additives: Renewable Fuel these test methods.
Standard Requirements for 2006) require petroleum distribu- 5.2 The use of glass and metal, in particular with closed
tors to add renewable ethanol to domestically sold gasoline to systems containing oxygen that are subjected to 700°C tem-
promote the nation’s growing renewable economy, with re- peratures pose their own safety concerns and care should be
quirements to identify and trace origin. taken to protect the operators from implosion/explosion of the
4.2 Method B utilizes Accelerator Mass Spectrometry glass tube. Material Safety Data Sheets should always be
(AMS) along with Isotope Ratio Mass Spectrometry (IRMS) followed with special concern for eye, respiratory, and skin
techniques to quantify the biobased content of a given product. protection. Radioactive 14C compounds should be handled and
Intsrumental error can be within 0.1-0.5 % (1 rsd), but empiri- disposed of in accordance with State and Federal Regulations.

3
 D6866 − 12
NOTE 1—Prior to D6866 - 11, this standard contained a Method A, carbon is quantitatively recovered as CO2. Weighed sample
which utilized LSC and CO2 absorption into a cocktail vial. Error was material shall be contained within a pre-cleaned quartz sample
cited as 615 % absolute due to technical challenges and low radiocarbon
counts. Empirical evidence now indicates error may be 620 % or higher
container, furnace-baked at 900°C for $2 h, and torch sealed at
in routine use. This method was removed in this revision due to the one end. Typically 2 mm OD/1 mm ID quartz tubing is
inapplicability of this low precision method to biobased analysis. sufficient, however any tubing configuration needed to accom-
5.3 In Method C, benzene is generated from the sample modate large sample volumes is acceptable.
carbon. Benzene is highly toxic and is an EPA-listed carcino- 8.3 The weighed sample shall then be transferred into an
gen. It must be handled accordingly, using all appropriate eye, appropriately sized quartz tube, typically 6 mm OD/4 mm ID.
skin, and respiratory protection. Samples must be handled and
disposed of in accordance with State and Federal regulations. 8.4 The sample, thus configured shall then be adapted to a
Other hazardous chemicals are also used, and must be handled vacuum manifold for evacuation of ambient air to a pressure
appropriately (see Material Safety Data Sheets for proper 101 Pa or less.
handling procedures). 8.5 If the material is known to be volatile or contains
volatile components, the sample material within the tube shall
METHOD B be frozen with liquid nitrogen to –196°C prior to evacuation.
6. Apparatus and Reagents The evacuated tube shall be torch sealed then combusted in a
temperature controlled furnace at 900°C for 2 to 4 h.
6.1 AMS and IRMS Apparatus:
6.1.1 A vacuum manifold system for with capabilities for air 8.6 After combustion, the quartz sample tube shall be scored
and non-condensable gas evacuation, sample introduction, to facilitate a clean break within a flexible hose portion of a
water distillation, cryogenic gas transfer, and temperature and “tube cracker” assembly adapted to the manifold. One example
pressure monitoring. The following equipment is required: configuration of a tube cracker is shown in the photo below.
6.1.2 Manifold tubing that is composed of clean stainless The materials are composed of stainless steel. Compression
steel and/or glass. fittings with appropriate welds are used to assemble the
6.1.3 Vacuum pump(s) capable of achieving a vacuum of individual parts. This and alternative assemblies are given in
101 Pa or less within the vacuum region. the References section (5,6,10,11).
6.1.4 Calibrated pressure transducers with coupled or inte- 8.7 With the manifold closed to the vacuum pump, the
grated signal response controllers. quartz tubing is cracked, the sample CO2 is liberated and
6.1.5 A calibrated sample collection volume with associated immediately cryogenically (with liquid nitrogen) transferred to
temperature readout. a sample collection bulb attached to a separate port on the
6.1.6 Clean quartz tubing for sample combustion and sub- manifold.
sequent gas transfer, quantification and storage.
6.1.7 A hydrogen/oxygen torch or other heating device 8.8 The contents of the sample collection bulb shall be
and/or gas for sealing quartz tubing. distilled to remove residual water using a dry ice/alcohol slurry
maintained at ca. −76°C. Simultaneously the sample CO2 gas
7. AMS and IRMS Reagents is released and immediately condensed in a calibrated volume.
7.1 A stoichiometric excess oxygen for sample combustion; 8.9 The calibrated volume is then closed and the CO2 shall
introduced into sample tube as either a pure gas or as solid equilibrate to room temperature.
copper (II) oxide.
8.10 Recovery shall be determined using the ideal gas law
7.2 A stoichiometric excess of silver, nominally 30 mg, relationship.
introduced into sample tube for the removal of halogenated
species. 8.11 The sample shall be transferred to a borosilicate break
seal tube for storage and delivery to an AMS facility for
7.3 A −76°C slurry mixture of dry ice (frozen CO2) and analysis of 14C/12C and 13C/12 C isotopic ratios.
alcohol distillation and removal of sample water.
7.4 Liquid nitrogen. 9. Analysis, Interpretation, and Reporting

8. Sample Preparation 9.1 14C/12C and 13C/12C isotopic ratios are measured using
accelerator mass spectrometry. The isotopic ratios of 14C/12C
8.1 Method B is a commonly used procedure to quantita- and 13C/12C are determined relative to the appropriate primary
tively combust the carbon fraction within product matrices of reference material, that is, SRM 4990c and RM 8544, for 14C
varying degrees of complexity. The procedure described here and 13C, respectively. Zero percent 14C represents the entire
for Method B is recommended based on its affordability and lack of 14C atoms in a material thus indicating a fossil (for
extensive worldwide use. Nevertheless, laboratories with alter- example, petroleum based) carbon source. One hundred per-
native instrumentation such as continuous flow interfaces and cent 14C, after correction for the post-1950 bomb injection
associated CO2 trapping capabilities are equally suitable pro- of 14C into the atmosphere, likewise indicates an entirely
vided that the recovery of CO2 is quantitative, 100 6 5 %. modern carbon source. The percent modern carbon can be
8.2 Based on the stoichiometry of the product material, slightly greater than 100 % due to the continuing, but
sufficient sample mass shall be weighed such that 1-10 mg of diminishing, effects of the 1950s nuclear testing programs.

4
 D6866 − 12
Because all sample 14C activities are referenced to a “pre- 10.10 Counting efficiency and background optimization
bomb” standard, all percent modern carbon values must be should be performed using a suitable reference standard (for
multiplied by 0.95 to correct for the bomb carbon and to example, NIST oxalic acid or Australian National University
subsequently obtain the true biobased content of the sample. (ANU) sucrose) using the same reagents and counting param-
References for reporting carbon isotopic ratio data are given in eters as the samples.
Refs (27,3) for 14C and 13C, respectively.
10.11 Counting efficiency (E) shall be determined by divid-
9.2 All percent modern carbon (pMC) values obtained from ing the measured cpm by the known dpm, and multiplying this
the radiocarbon analyses must be corrected for isotopic frac- by 100 to obtain the counting efficiency as a percentage. For
tionation (28) using stable isotope data (13C/12C ratios) ob- example, for the Oxalic Acid I standard, E = (cpm/g Oxalic
tained on CO2 derived from combustion of the sample. Do not Acid/ 14.27 dpm/g) × 100, where E = counting efficiency in %,
determine 13C/12C ratios on the raw product material itself, cpm/g Oxalic Acid is the net activity per gram measured for the
since that approach can lead to erroneous results in some cases. oxalic acid after subtracting background, and 14.27 dpm/g is
the absolute value of the NIST “OxI” reference standard. The
9.3 Biobased content values that exceed 100 % should be
NIST “OxII” standard (SRM 4990C) has a slightly different
reported as having a biobased content of 100 %. A biobased 14
C activity level. ANU sucrose (NIST SRM 8542) can be
content that is greater than 103 % suggests that either an
used as a suitable standard in place of oxalic acid.
analytical error occurred, or that the source of biobased carbon
is more than several years old. In such cases, the analyst should 10.12 Counting interference concerns that must be ad-
discuss the product with the manufacturer to determine if dressed as part of specific instrument calibration and normal-
re-analysis of the product is warranted. Re-analysis would be ization include luminance, chemical or color quench, static
warranted if the biobased carbon is less than two or three years electricity, random noise, temperature, and humidity variability
old, in which case an analytical error would be suspected. (13).
METHOD C 10.13 Alternate regions of interest parameters may be used
based upon testing of 20, or more, 6-h counts of the same
10. Detailed Requirements reference (STDCT) standard that record the raw data and
NOTE 2—Acceptable tolerance levels of 65 % are standard to this spectrum for keV regions of interest 4 through 96. Optimal
method unless otherwise stated. counting conditions should be established by maximizing the
Figure of Merit (E2/bkg) values to obtain the highest count
10.1 Low level liquid scintillation analyzers with active
efficiency and the lowest background and other interference.
shielding that can produce consistent background counts of less
Counting efficiency of less that 60 % is unacceptable and can
than 5 dpm.
be improved by LSC instrument optimization and sample/
10.2 Anticoincidence systems such as two and three photo- reagent compatibility or shielding improvements.
multiplier tubes (multidetector systems).
10.14 Samples will be equilibrated with reference standards
10.3 Coincidence circuits. under identical conditions of time and temperature.
10.4 Software and hardware that include thresholds and 10.15 Samples will be counted for a minimum of 10 h with
statistics, pulse rise and shape discrimination, and three- region of interest (ROI) channels including ROI energy levels
dimensional spectrum analysis. of 0-155 keV such that E2/B is 1000 or higher in 20 to 120-min
subsets with raw data saved to disk for later statistical analysis
10.5 Use of external and internal standards must be used in
and documentation of stable counting conditions.
LSC operation.
10.16 Before commercial testing, laboratories that intend to
10.6 Optimized counting regions to provide very low back-
implement this method must participate in an interlaboratory
ground counts while maintaining counting efficiency greater
comparison study to assess between laboratory reproducibility.
than 60 % of samples 0.7 to 1.5 g in clean, 3-mL, 7-mL or
20-mL low potassium glass counting vials. Alternatively, clean
PTFE or quartz counting vials may be used in this method. 11. Apparatus and Reagents

10.7 No single LSC is specified for this method. However, 11.1 Benzene Synthesis Apparatus
minimum counting efficiency and control of background inter- 11.1.1 A benzene synthesis unit will be required to convert
ference is specified. Like all analytical instruments, LS coun- sample carbon to benzene. These units are commercially
ters require study as to their specific components and counting available, but can also be home-made if desired. Examples of
optimization. benzene synthesis units are discussed in (12) and (30).

10.8 Standardization of sample preparation is required. 11.2 LSC Apparatus

11.2.1 Liquid scintillation analyzer as described in Section
10.9 Standardization and optimization of clean sample 10.
vials, which must be made of either PTFE, quartz, or low-
11.2.2 Clean low potassium scintillation vials with a volume
potassium glass with PTFE tops. Sample vials may be either
of 3 mL, 7 mL, or 20 mL.
3-mL, 7-mL or 20-mL in volume. Plastic vials must not be used
for this method. 11.3 LSC and Benzene Synthesis Reagents

5
 D6866 − 12
11.3.1 High purity oxygen for converting sample carbon to 12.8 The Li2C2 is heated to about 900°C and placed under
CO2. Alternatively, technical grade oxygen can be used if vacuum for 15-30 minutes to remove any unreacted gases and
scrubbed with a suitable material such as Ascarite. to complete the Li2C2 synthesis reactions (27).
11.3.2 High purity nitrogen for combining with the oxygen 12.9 The Li2C2 is cooled to room temperature and gently
when combusting highly volatile samples. Alternatively, tech- hydrolyzed with distilled or de-ionized water to generate
nical grade nitrogen can be used is scrubbed with a suitable acetylene gas (C2H2) by applying the water in a drop-wise
material such as Ascarite. fashion to the carbide. The evolved acetylene is dried by
11.3.3 Cupric oxide wire for conversion of CO to CO2 when passing it through dry ice traps, and the dried acetylene in
combusting highly volatile samples with oxygen/nitrogen subsequently collected in liquid nitrogen traps.
blends.
11.3.4 Reagent grade powdered lithium or lithium rod (each 12.10 The acetylene gas is purified by passing it through a
packed in argon) for converting CO2 to lithium carbide phosphoric acid or potassium chromate (in sulfuric acid) trap to
(Li2C2). remove trace impurities, and by using dry ice traps to remove
11.3.5 Reagent grade potassium chromate (in sulfuric acid) water.
or phosphoric acid for purifying acetylene gas. 12.11 The C2H2 gas is catalyzed to benzene (C6H6) by
11.3.6 Suitable catalyst material such as a Si2O3/Al2O3 bleeding the acetylene onto a chromium catalyst which has
substrate activated with either chromium (as Cr2O3) or vana- been preheated to $90°C, or onto a vanadium catalyst (the
dium (as V2O5) for converting acetylene gas to benzene (23). later activates at ambient temperature). In the former case, the
11.3.7 Scintillation cocktail. reaction is cooled with a water jacket to avoid decomposition
11.3.8 De-ionized or distilled water for hydrolysis of Li2C2 from excessive heat generated during the exothermic reaction.
to acetylene gas. 12.12 The benzene is thermally evolved from the catalyst at
70-110°C and then collected under vacuum at roughly -78°C.
12. Sample Preparation and Analysis The benzene is then frozen until it is counted. Radon can be
12.1 Tolerance of 65 % is to be assumed unless otherwise removed by pumping on the benzene while it is at dry ice
stated. temperatures.
12.2 Standard procedures are to be employed for the con- 12.13 The 14C content shall be determined in a LSC with
version of original sample material to benzene using the liquid optimization of the instrument as described in Section 10.
scintillation dating technique (12). Either single vial counting or “chain” counting is acceptable.
12.3 Based on the stoichiometry of the product material, 12.14 Radiocarbon activity in the sample is to be deter-
sufficient sample mass shall be weighed such that quantitative mined by “benzene cocktail” analysis, consisting of a scintil-
recovery of the carbon would theoretically yield 1.00 to 4.00 g lator plus sample benzene, in constant volume and proportion.
of carbon for conversion to benzene. A recommended scintillator is butyl-PBD or PPO/POPOP
dissolved in toluene or equivalent (13) and(16). Alternatively,
12.4 The carbon within each sample shall first be combusted some scintillators (including butyl-PBD) can be added to the
to CO2 by placing the sample in a closed system which is benzene as a solid with good results.
purged or evacuated of air.
12.15 Standard methods consist of counting a cocktail
12.5 The system is then purged several times with pure containing sample benzene plus a scintillation solution. For
nitrogen. After verifying the integrity of the closed system, the example, a cocktail might contain 4-mL sample benzene plus
sample is bathed in 100 % oxygen (non-volatile samples) or a 0.5-mL scintillation solution. In this example, if 4 mL of
mixture of nitrogen and oxygen (volatile samples) and ignited. sample benzene is not available, reagent grade (99.999% pure)
Samples ignited using a nitrogen/oxygen mix must pass thiophene-free benzene can be added to bring the sample
through a cupric oxide furnace at 850°C to avoid carbon loss to volume to 4 mL. Larger or smaller volumes may be utilized
CO. The generated sample CO2 is collected using liquid depending upon the configuration of the specific laboratories
nitrogen cold traps. If desired, the CO2 can be passed through counting protocols.
a series of chemical traps to remove various contaminants prior
to cryogenic collection of the CO2 (12). 12.16 Scintillation counters are to be monitored for back-
ground and stability with traceable documentation.
12.6 As an alternative combustion approach for volatile
materials, the samples can be combusted in a bomb that is 12.17 Should anomalies appear during sample counting, the
pressurized with oxygen to 300-400 psi. The CO2 generated in benzene is to be re-measured in another counter to verify the
the bomb is subsequently released to a dry ice trap for moisture activity, or the sample must be completely re-analyzed.
removal, followed by a liquid nitrogen cold trap for CO2 12.18 Traceable quench detection should be performed on
collection. each sample to ensure benzene purity. In the event the sample
12.7 The collected CO2 is reacted with a stoichiometric is substantially quenched, the data should be discarded and the
excess (3:1 lithium:carbon ratio) of molten lithium which has sample should be re-analyzed.
been preheated to 700°C. Li2C2 is produced by slowly bleeding 12.19 Measurements are to be made on an interval basis
the CO2 onto the molten lithium in a stainless steel vessel (or (usually 50 or 100 minutes) to allow statistical analysis of the
equivalent) while under a vacuum of #135 mPa. measurement.

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12.20 Prior to removing the sample from the counter, multiplied by 0.95 (as of 2010) to better reflect the true
stability is to be verified and the data scrutinized for anomalies. biobased content of the sample.
If the distribution does not closely follow Gaussian statistics, 13.4 Biobased content values that exceed 100 % should be
the sample should be transferred and counted in another reported as having a biobased content of 100 %. A biobased
counter for verification, or the sample should be completely content that is greater than 103 % suggests that either an
re-analyzed. analytical error occurred, or that the source of biobased carbon
12.21 Counting should be performed as needed to obtain a is more than several years old. In such cases, the analyst should
precision of 2 % or better. discuss the product with the manufacturer to determine if
re-analysis of the product is warranted. Re-analysis would be
12.22 Calculation of the data should be performed only after
warranted if the biobased carbon is less than two or three years
cross-checking all transcribed numbers, synthesis records,
old, in which case an analytical error would be suspected.
cocktail preparation, counting data, and counting analysis.
12.23 Any unused sample material shall be maintained at SPECIAL PROCEDURES FOR CARBONATE-
the laboratory for potential re-analysis for a minimum of 180 BEARING PRODUCTS
days. The sample will then be disposed of in accordance with
state and federal regulations. 14. Background
14.1 Some biobased products contain substantial amounts
12.24 Because of problems in storing benzene over ex-
of inorganic carbonates. When using the sample preparation
tended periods of time, it may be necessary to re-distill (to
procedures stipulated in Methods B and C, some or all of the
remove scintillant) and re-weigh the benzene if re-analysis is
carbon associated with the inorganic carbonates could be
desired at a later date. Alternatively, a fresh portion of the
included in the analysis. However, based on the USDA
biobased product can be processed to obtain a fresh benzene
definition of “biobased content,” the biobased content deter-
sample.
mination must be based only on the organic carbon. By
NOTE 3—The benzene derived from the sample carbon is toxic and is a
known carcinogen. Special handling and disposal procedures will be definition, the carbon associated with inorganic carbonates is
required. not to be included in the “biobased content” determination for
any given product, regardless of whether those carbonates
13. Interpretation and Reporting contain 14C. Therefore, special procedures must be used to
analyze biobased products that contain detectable (using pro-
13.1 The counts shall be compared, directly or through cedures described in 15.1) levels of inorganic carbonates. The
secondary standards, to the 14C oxalic acid SRM 4990c (or procedures described herein are applicable to solid materials.
other suitable standard), with stated uncertainties. Significantly
lower 14C counts indicate the presence of 14C-depleted carbon. 15. Sample Analysis and Reporting
The lack of any 14C counts in a material indicates a fossil (for
example, petroleum based) carbon source. A sample that has 15.1 If it is not known whether or not a biobased product
the same 14C activity level (after correction for the post-1950 contains inorganic carbonates, the product must be checked for
bomb injection of 14 C into the atmosphere) as the oxalic acid the presence of carbonates before any biobased content deter-
standard is 100 % biobased and signifies an entirely modern minations are performed. The presence of carbonates can be
carbon source. The inherent assumption is that all of the adequately detected in powdered samples using 10 % HCl and
organic components within the analyzed material are either seeing if the sample effervesces. Even low (for example, 1 %)
fossil or present day in origin. concentrations of carbonates can be readily detected by squirt-
ing 2-3 mL of 10 % HCl onto at least one gram of the
13.2 All percent modern carbon (pMC) values obtained powdered sample to see if the acidified sample effervesces
from the radiocarbon analyses must be corrected for isotopic (indicating the presence of carbonates). However, a limitation
fractionation (28) after performing stable carbon isotope analy- to this approach is that it assumes that the carbon content of the
ses (13C/12C ratios). The stable isotope analyses must be sample is reasonably high. If the carbon content of a sample is
performed on a portion of the CO2 derived from the combus- low (for example, 10 % or less), then even very small concen-
tion of the sample. trations of inorganic carbonate in the sample could constitute a
13.3 The percent modern carbon can be greater than 100 % significant fraction of the total carbon, yet the carbonate may
because of the continuing but diminishing effects of the 1950s not be detectable using the acidification procedure. This could
nuclear testing programs, which resulted in a considerable incur significant analytical errors if suitable corrections are not
enrichment of 14C in the atmosphere. The decrease in 14C from made for the inorganic carbon. This approach also assumes that
the bomb testing programs has been nonlinear. Although it the carbonate particles are not coated with a material that is not
continues to decrease by a small amount each year, the quickly dissolved in the dilute acid. Judgment calls are often
current 14C activity in the atmosphere has not reached the 1950 required by the analyst in such cases. If there is some question
level of 13.56 dpm per gram carbon that is defined as 100 as to whether or not a product contains significant levels of
pMC. Because all sample 14C activities are referenced to a inorganic carbonate, the product manufacturer should be con-
“pre-bomb” standard, and because nearly all new biobased tacted to address this issue.
products are produced in a post-bomb environment, all pMC 15.2 Two procedural options are applicable for the removal
values (after correction for isotopic fractionation) must be of carbonate carbon from the final biobased result.

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 D6866 − 12
15.2.1 Carbonate Option A (Carbonate Subtraction) in- determine its pMC value. This step is necessary since, by
volves making measurement of the total organic carbon (TOC), USDA definition, the biobased content of a biobased product
total inorganic carbon (TIC) and the associated radiocarbon must not include inorganic material. Therefore, with the
content of each. It is recommended that only laboratories exceptions noted above, any radiocarbon associated with the
having very high precision capabilities for quantifying TOC inorganic carbonates must be excluded from the reported
and TIC and the associated radiocarbon content of each use this biobased content value for that product.
method. Precision loss in the calculation of biobased content 15.6 Using the procedures described above, the mass frac-
will occur as the percentage of carbonate carbon to total carbon tions of the CO2 associated with the total sample (organic
in the product increases. material plus the inorganic carbonate) and with the carbonate
15.2.2 Carbonate Option B (Acid Residue Combustion) are known. The pMC (percent modern carbon) values associ-
involves making a single measurement on the soluble and ated with the CO2 from the total sample and with just the
insoluble organics remaining within an acidic solution follow- inorganic carbonate fraction are also known. Therefore, the
ing acid digestion of the product. It is recommended only for pMC associated with only the organic matter can be calculated
laboratories having qualified expertise in acid/base chemistry as follows:
and wet combustion.
~ pMCtotal! 2 ~ Mass Fraction Carbonate! ~ pMCcarbonate!
pMCorganic 5
CARBONATE OPTION A (CARBONATE Mass Fraction Organic
SUBTRACTION) (1)
15.3 Samples that contain carbonates require special proce- 15.7 As an example, assume that the CO2 derived from the
dures and may have to be analyzed using a two-part analytical entire sample is 50.0 pMC, and that the CO2 derived from the
procedure using either benzene synthesis or AMS (the ASTM carbonate fraction is 5.0 pMC. Furthermore, assume that 40 %
CO2 cocktail method is not suitable for analyzing carbonate- of the CO2 generated during sample combustion (that is,
bearing samples). Also, no sealed vessels (for example, a Parr analysis of the whole sample) is derived from the carbonates.
oxygen bomb) are to be used during the combustion of The pMC associated with only the organic fraction of the
carbonate-containing samples when preparing them for analy- sample is then calculated as follows:
sis by benzene synthesis or AMS. This is because a CO2 -rich
~ 50.0 pMC! 2 ~ 0.40! ~ 5.0 pMC!
atmosphere may inhibit the decomposition of carbonates and pMCorganic 5 5 80.0 pMC (2)
0.60
can shift carbonate decomposition temperatures to much higher
levels. This could potentially lead to errors in the biobased 15.8 As noted in Methods B and C, the pMC values must be
content determination. multiplied by 0.95 in order to correct for “bomb” carbon.
Therefore, in this case, the biobased content would be reported
15.4 First, a sample of the biobased product shall be
as (80.0) (0.95), or 76 % biobased content (values should
analyzed in accordance with standard procedures (but avoiding
always be rounded to the nearest 1 % biobased content).
the use of sealed vessels). This will provide the percent modern
carbon (pMC) value associated with the entire sample (carbon 15.9 The biobased content value obtained from this two-
associated with the organic material plus the carbonates). As step procedure is expected to be accurate to within 64 %
part of this procedure, the amount of CO2 generated from the (absolute). This takes into account the fact that the reported
sample must be measured and recorded. If the biobased content biobased content value is a result of two separate radiocarbon
of the entire sample is determined to be at least 97 %, then the measurements, which each have an analytical uncertainty of
presence of inorganic carbonates does not significantly affect about 63 % absolute.
the accuracy of the biobased content determination, and no
CARBONATE OPTION B (ACID RESIDUE
further analyses are required. If the biobased content is less
COMBUSTION)
than that, then proceed to 15.5.
15.5 Next, a fresh sample portion of the biobased product is 15.10 In comparison to the Carbonate Subtraction method,
acidified with diluted (for example, 10 %) HCl or heated (for only one analysis is required using the Acid Residue Combus-
example, 70-90°C) concentrated H3PO4. The CO2 generated tion method. In this method, the product is crushed, digested in
during the sample acidification is collected and quantified. phosphoric acid (H3PO4) and the residue solution is com-
Based on the amounts of CO2 generated per unit weight of busted. Organic carbon bearing species within the solution are
sample (determined in 15.4 and 15.5), the percentage of the oxidized to CO2 suitable for biobased content determination.
total carbon that is present as carbonates can be calculated. If Note that due to the complicated nature of combusting an acid
the inorganic carbon is found to constitute less than 3 % (wt) of solution, small quantities are recommended applicable to
the total carbon in the sample, then no additional analyses are analysis by way of Method B.
required. In that event, the presence of inorganic carbonates 15.11 First, in the case of solid material, surface area is
will have little or no impact on the accuracy of the biobased increased as necessary via grinding, pulverizing or crushing.
content determination, and the biobased content can be re- This is especially important in the case of bioplastics or other
ported based on the total carbon in the sample. If the inorganic materials which may encapsulate carbonate grains. It is impor-
carbon constitutes more than 3 % (wt) of the total carbon in the tant to produce sub-millimeter or sub-micron particle sizes to
sample, then the CO2 generated during the acidification pro- ensure maximum exposure to carbonate surfaces. The powder
cedure must be analyzed for radiocarbon content in order to is then poured into a glass vessel suitable for evacuation of all

8
 D6866 − 12
air, to –30 psi (standard rotary vacuum pump range). [H3PO4] cable to determining the biobased content of gases where the
is added to the vessel (in the absence of air) and observation is carbon is already in gaseous form. This includes gaseous
made for the presence or absence of effervescence. If efferves- emissions from electric utility boilers, waste incinerators, and
cence is observed, the material is identified to contain inor- syngas plants. To avoid confusion in terminology, results
ganic carbon. In the case of aqueous solution, [H3PO4] is added obtained for gaseous emissions should be reported as “biogenic
directly to the solution under observation for effervescence. carbon content” or “biogenic CO2 content,” not “biobased
NOTE 4—It is useful to know the pH of the solution prior adding the
carbon content” since inorganic carbon cannot be eliminated
acid. It is understood caution, best laboratory practice and safety is used from the final result.
in adding the acid. High pH solutions can get very hot and react strongly. 16.2 The analytical methods for determining biobased con-
If effervescence is observed, carbonate is indicated.
NOTE 5—Some materials may “boil” with the addition of the acid. If it
tent are also directly applicable to the determination of
can be determined the effervescence is not related to the generation of renewable carbon content of solid fuels combusted in waste-
CO2, it is reasonable to assume the material does not contain carbonate to-energy plants and municipal incinerators. In this case, the
and the product can be analyzed as such. If such a determination cannot source of the carbon is very often the same as described above
be made, it is reasonable to assume the material does contain carbonate for gaseous emission, but with the solid fuel itself being the
and combustion of the residual solution is warranted.
material submitted for analysis. Additionally, applicability of
15.12 Next, the acid+product solution is combusted. In the result is related to total CO2 emissions, including both
some cases, it may be necessary to repeat the above steps to organic and inorganic sourced carbon. Therefore, the overall
produce an appropriate size sample for combustion. If for analytical methods described in this standard are applicable to
example, the glass vessel used for the test was quartz or Vycor, determining the renewable content of solid fuels where the
the combustion system can be designed to incorporate it in renewable carbon relative to the total carbon (versus total
such a way that the original solution can be combusted directly organic carbon) is the value of interest. As such, all analytical
without transfer. In any case, the solution to be used is methods are the same, with the exclusion of consideration of
subjected to an active flow of oxygen (100 % or N2 diluted inorganic carbon contribution. Therefore, to avoid confusion in
dependent upon the flammability/volatility of the solution) and terminology, results obtained for any material containing
heated. Evolved CO2 is collected in a liquid nitrogen trap for inorganic carbonates should be reported as “biogenic carbon
subsequent analysis by Method B. The most volatile/least content,” not “biobased carbon content” since inorganic carbon
pyrolizable components will evolve first. The system should be is included in the final result. Examples of such materials are
designed with a furnace at >800+C packed with quartz wool or solid fuels, municipal solid waste (MSW) and precipitated
turnings downstream from the sample to combust vaporized calcium carbonate (PCC).
organic compounds. Upon removal of volatile components, it
is common to see solids precipitate, burn or pyrolize as the 17. Sample Analysis and Reporting
heating continues. In the final steps of combustion, heat should 17.1 Gas sampling issues are not addressed in these test
be applied to the vessel containing the remnants of the product methods. However, once a gas sample is collected, it can be
(minerals, ash, or highly pryolizable organic compounds) to processed in accordance with the post-combustion procedures
temperatures such that no organic constituents (usually black) already stipulated in this method.
may remain uncombusted.
17.2 The age of the biomass used in industrial processes
NOTE 6—It is common for the caustic nature of the combusted solution will affect the accuracy of the biobased content measurement,
to damage the heated glass and components beyond repair. As such, it is and there will likely be cases where the age of the biomass is
often necessary to replace the system with new glass components after not accurately known. The results are anticipated to be accurate
each sample.
to within 5 % biobased content if the biorenewable carbon
15.13 The biobased content value obtained from this acid components are within 10 years of present day and if the
residue combustion procedure is expected to be accurate to samples are analyzed by AMS. The accuracy of the measure-
within 63 % (absolute) since it involves just a single analysis ment will increase as the age of the biorenewable carbon
step rather than the two-step procedure described for the components diminishes.
carbonate subtraction approach.
18. Precision and Bias
ANALYSIS OF GASEOUS EMISSIONS AND BULK 18.1 The precision and bias of Methods B and C from any
MATERIALS CONTAINING RENEWABLE CARBON reporting laboratory will be deemed acceptable if it can be
shown that the data are traceable to the primary standards and
16. Background
within the uncertainties stated in 4.2 and 4.3.
16.1 The initial step in determining the biobased content of
any solid or liquid sample is to convert the sample carbon to 19. Keywords
gaseous CO2 (any CO resulting from incomplete combustion 19.1 accelerator mass spectrometry; biobased; 14C (carbon-
during this step is also oxidized to CO2). Therefore, the overall 14); carbon dating; isotope ratio mass spectrometry; liquid
analytical methods described in this standard are also appli- scintillation counting; new carbon; old carbon

9
 D6866 − 12

APPENDIX

(Nonmandatory Information)

X1. FIGURES

FIG. X1.1 Example of a Gas Transfer Manifold

10
 D6866 − 12

FIG. X1.2 Example of a Flexible Glass Tube Cracker

11
 D6866 − 12

FIG. X1.3 Example of a Flexible Tube Cracker with Three-way Valve

12
 D6866 − 12
REFERENCES

(1) Ramani Narayan, Biobased and Biodegradable Polymer Materials: LSC Application,” Packard BioScience Company, Meriden, CT,
Rationale, Drivers, and Technology Exemplars, ACS (an American 1997.
Chemical Society Publication) Symposium Ser.,939, June 2006 (18) L’Annuniziata, M. F., Handbook of Radioactivity Analysis, Aca-
(2) Alessio, M., Allegri, L., Bella, F., and Improta, S., “Study of demic Press, New York, 1998.
Background Characteristics by Means of High Efficiency Liquid (19) L’Annuniziata, M. F., “The Detection and Measurement of
Scintillation Counter,” Nucl Instum. Methods Phys. Res., Vol 137, Radionuclides,” Isotopes and Radiation in Agricultural Sciences,
1976, pp. 537-543. 1984, pp. 141-231.
(3) Allison, C. E., Francy, R. J., and Meijer, H. A. J., “Reference and (20) Noakes, J. E., “Low-Level Liquid Scintillation Counter Array with
Intercomparison Materials for Stable Isotopes of Light Elements,” Computerized Data Acquisition and Age Calculation Capabilities
International Atomic Energy Agency, Vienna, Austria, IAEA- for 14C Dating,” Radiocarbon, Vol 37, No. 2, 1995, pp. 773-779.
TECHDOC-825, 1995. (21) Noakes, J. E., “Consideration for Achieving Low Level Radioactiv-
(4) Anderson,
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R., and Cook, G. T., “Scintillation Cocktail Optimization ity Measurements with Liquid Scintillation Counters,” Liquid Scin-
for C Dating Using the Packard 2000 CA/LL and 2260 SL,” tillation Counting, Crook, M. A., and Johnson, P., Eds., Heyden,
Radiocarbon, Vol 33, 1991, pp. 1-7. London, Vol 4, 1977, pp. 189-206.
(5) Caldwell, W. E., Odom, J. D., and Williams, D. F., “Glass-sample (22) Noakes, J. E., and Valenta, R. J., “Low Background Liquid Scintil-
Tube Breaker,” Anal. Chem., Vol 55, 1983, pp. 1962-1963. lation Counting Using an Active Sample Holder and Pulse Discrimi-
(6) Coleman, D. D., “Tube Cracker for Opening Sealed Samples in Glass nation Electronics,” Radiocarbon, Vol 31, 1989, No. 3, pp. 332-341.
Tubing,” Anal. Chem., Vol 55, 1983, pp. 1175-1176. (23) Noakes, J. E., “Low Temperature Conversion of Acetylene to Pure
(7) Cook, G. T., Naysmith, P., Anderson, R., and Harkness, D. D., Benzene,” U.S. Patent #3,365,510, January 23, 1968.
“Performance Optimization of the Packard 2000 CA/LL Liquid (24) Polach, H., “Liquid Scintillation 14C Spectrometry: Errors and
Scintillation Counter for 14 C Dating,” Nucl. Geophys., Vol 4, 1990a, Assurances,” Radiocarbon, Vol 31, No. 3, 1989, pp. 327-331.
pp. 241-245. (25) Qureshi, R. M., Fritz, P., and Dsimmie, R. J., “The Use of CO2
(8) Currie, L. A., Stafford, T. W., Sheffield, A. E., Wise, S. A., Fletcher, R. Absorbers for the Determination of Specific 14C Activities,” Int. J.
A., Donahue, D. J., Jull, T. J. T., and Linick, T. W., “Microchemical Appl. Radiat. Isot., Vol 36, No. 2, 1985, pp. 165-170.
and Molecular Dating,” Radiocarbon, Vol 31, No. 3, 1989, pp. (26) Qureshi, R. M., Aravena, R., Fritz, P., and Drimmie, R., “The CO2
448-463. Absorption Method as an Alternative to Benzene Synthesis Method
(9) Currie, Lloyd A., Klinedinst, Donna B., Burch, R., Feltham, N., and for 14C Dating,” Appl. Geochem., Vol 4, 1989, pp. 625-633.
Dorsch, R., “Authentication and Dating of Biomass Components of (27) Roessler, N., Valenta, R. J., and van Cauter, S., “Time-resolved
Industrial Materials; Links to Sustainable Technology,” Nuclear Liquid Scintillation Counting,” Liquid Scintillation Counting and
Instruments and Methods in Physics Research, Section B, Vol 172, Organic Scintillators, Ross, H., Noakes, J. E., and Spaulding, J. D.,
2000, pp. 281-287. Eds., Lewis Publishers, Chelsea, MI, 1991, pp. 501-511.
(10) Levin, I., and Kromer, B., “Twenty Years of Atmospheric 14CO2 (28) Stuiver, M., and Polach, “Reporting of 14C Data,” Radiocarbon, Vol
Observations at Schauinsland Station, Germany,” Radiocarbon, Vol 19, No. 3, 1977, pp. 355-363.
39, No. 2, 1997, pp. 205-218. (29) Takiue, M., Natake, T., and Fujii, H., “Liquid Scintillation Radioas-
(11) DesMarais, D. J., and Hayes, J. M., “Tube Cracker for Opening say for Low-activity Beta Emitter Mixtures by the Method of Least
Glass-sealed Ampoules Under Vacuum,” Anal. Chem., Vol 48, 1976, Squares,” J. Radioanal. Nucl. Chem. Lett., Vol 200, 1995, pp.
pp. 1651-1652. 247-258.
(12) Gupta, S. K. and Polach, H. A., Radiocarbon Dating Practices at (30) Tamers, M. A., “Chemical Yield Optimization of Benzene Synthesis
ANU: Handbook, Radiocarbon Dating Research, Garran, Australia, for Radiocarbon Dating,” Int. J. Appl. Radiat. Isot., Vol 26, No. 10,
1985, pp. 1-173. 1975, pp. 676-682.
(13) Horrocks, D., ed., Applications of Liquid Scintillation Counting, (31) Thomson, J., and Burns, D. A., “Environmental Sample Preparation
Academic Press, New York, 1974. for LSC,” Counting Solutions CS-004, Packard Instrument
(14) Kennedy, H., and Kennedy, D. P., “Simplified Tube Cracker for Company, Meriden, CT, 1996a; Thomson , J., and Burns, D. A.,
Opening Samples Sealed in Glass Tubes While Under Vacuum,” “LSC Sample Preparation by Solubilization,” Counting Solutions
Analy. Proc. Analyt. Comm., Vol 31, 1994, pp. 299-300. CS-003, Packard Instrument Company, Meriden, CT, 1996b.
(15) Kessler, M. J., Ed., “Liquid Scintillation Analysis—Science and (32) Thomson, J., “Counting Aqueous Samples by LSC,” Counting
Technology,” Packard publication, Packard Instrument Company, Solutions CS-005, Packard Instrument Company, Meriden, CT, 1997.
Meriden, CT, 1989. (33) Thomson, J., and Burns, D. A., “Radio-carbon Dioxide (14CO2)
(16) Koba, M., “Improved Results Using Higher Ratios of Scintillator Trapping and Counting,” Counting Solutions CD-001, Packard
Solution to Benzene in Liquid Scintillation Spectrometry,” Instrument Company, Meriden, CT, 1994.
Radiocarbon, Vol. 42, No. 2, 2000, pp. 295-303. (34) Winyard, R., Lutkin, J. E., and McGeth, G. W., “Pulse Shaped
(17) L’Annuniziata, M. F., “Efficiency Tracing DPM (ET-DPM) and Discrimination in Inorganic and Organic Scintillators,” Nucl. In-
Direct-DPM-Instrument Performance Data. Counter Intel. Tri-Carb strum. Methods Phys. Res., Vol 95, 1971, pp. 141-154.

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SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue (D6866 - 11)
that may impact the use of this standard. (April 1, 2012)

(1) Revised Sections 15 and 16.

Committee D20 has identified the location of selected changes to this standard since the last issue (D6866 - 10)
that may impact the use of this standard. (April 1, 2011)

(1) Deleted previous 4.2. (5) Revised 5.2.

(2) Revised current 4.2, which was previously 4.3. (6) Added Note 1.
(3) Revised current 4.3, which was previously 4.4. (7) Deleted “Method A” from the standard.
(4) Deleted previous 4.5 and renumbered remainder of Section
4.

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14