Designation: D 6866 – 05

Standard Test Methods for

Determining the Biobased Content of Natural Range
Materials Using Radiocarbon and Isotope Ratio Mass
Spectrometry Analysis1
This standard is issued under the fixed designation D 6866; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope* 3.2 Terminology D 883 should be referenced for terminol-

1.1 These test methods do not address environmental im- ogy relating to plastics. Although an attempt to list terms in a
pact, product performance and functionality, determination of logical manner (alphabetically) will be made as some terms
geographical origin, or assignment of required amounts of require definition of other terms to make sense.
biobased carbon necessary for compliance with federal laws. 3.3 Definitions:
1.2 These test methods are applicable to any product con- 3.3.1 dpm—disintegrations per minute. This is the quantity
taining carbon-based components that can be combusted in the of radioactivity. The measure dpm is derived from cpm or
presence of oxygen to produce carbon dioxide (CO2) gas. counts per minute (dpm = cpm − bkgd / counting efficiency).
1.3 These test methods make no attempt to teach the basic There are 2.2 by 106 dpm / uCi (13,16).3
principles of the instrumentation used although minimum 3.3.2 dps—disintegrations per second (rather than minute as
requirements for instrument selection are referenced in the above) (13,16).
References section. However, the preparation of samples for 3.3.3 scintillation—the sum of all photons produced by a
the above test methods is described. No details of instrument radioactive decay event. Counters used to measure this as
operation are included here. These are best obtained from the described in these test methods are Liquid Scintillation
manufacturer of the specific instrument in use. Counters (LSC) Bq (13,16).
1.4 Currently, there are no ISO test methods that are 3.3.4 specific activity (SA)—refers to the quantity of radio-
equivalent to the test methods outlined in this standard. activity per mass unit of product, that is, dpmh % (13,16).
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 (13).
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.
3.3.7 accelerator mass spectrometry (AMS)—an ultra-
2. Referenced Documents sensitive technique for measuring naturally occurring radio
2.1 ASTM Standards: 2 nuclides, in which sample atoms are ionized, accelerated to
D 883 Terminology Relating to Plastics high energies, separated on basis of momentum, charge, and
mass, and individually counted in Faraday collectors. This high
3. Terminology energy separation is extremely effective in filtering out isobaric
3.1 The definitions of terms used in these test methods are interferences, such that AMS may be used to measure accu-
referenced in order that the practitioner may require further rately the 14C abundance to a level of 1 in 1015. At these levels,
information regarding the practice of the art of isotope analysis uncertainties are based on counting statistics through the
and to facilitate performance of these test methods. Poisson distribution (7,8).
3.3.8 background radiation—the radiation in the natural
environment; including cosmic radiation and radionuclides
1
These test methods are under the jurisdiction of ASTM Committee D20 on present in the local environment, for example, materials of
Plastics and are the direct responsibility of Subcommittee D20.96 on Environmen- construction, metals, glass, concrete (1,3,6,7,13-18).
tally Degradable Plastics and Biobased Products.
Current edition approved March 1, 2005. Published April 2005. Originally
3.3.9 coincidence circuit—a portion of the electronic analy-
approved in 2004. Last previous edition approved in 2004 as D 6866 - 04a. sis system of a Liquid Scintillation Counter which acts to reject
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.

1
 D 6866 – 05
pulses which are not received from the two Photomultiplier quantitatively comparing certain aspects of instrument and
Tubes (that count the photons) within a given period of time cocktail performance and the term is frequently used to
and are necessary to rule out background interference and compare efficiency and background measures (13,16,19).
required for any LSC used in these test methods (6,13,16). 3.3.20 fluorescence—the emission of light resulting from
3.3.10 coincidence threshold—the minimum decay energy the absorption of incident radiation and persisting only as long
required for a Liquid Scintillation Counter to detect a radioac- as the stimulation radiation is continued (13,16,24).
tive event. The ability to set that threshold is a requirement of 3.3.21 fossil carbon—carbon that contains essentially no
any LSC used in these test methods (13,16). radiocarbon because its age is very much greater than the 5730
3.3.11 contemporary carbon—a direct indication of the year half-life of 14C (7,8).
relative contributions of fossil carbon and “living” biospheric
3.3.22 half-life—the time in which one half the atoms of a
carbon can be expressed as the fraction (or percentage) of
particular radioactive substance disintegrate to another nuclear
contemporary carbon, symbol fC. This is derived from fM
form. The half-life of 14C is 5730 years (7,13,24).
through the use of the observed input function for
atmospheric 14C over recent decades, representing the com- 3.3.23 intensity—the amount of energy, the number of
bined effects of fossil dilution of 14C (minor) and nuclear photons, or the numbers of particles of any radiation incident
testing enhancement (major). The relation between fC and fM is upon a unit area per unit time (13,16).
necessarily a function of time. By 1985, when the particulate 3.3.24 internal standard—a known amount of radioactivity
sampling discussed in the cited reference the fM ratio had which is added to a sample in order to determine the counting
decreased to ca. 1.2 (7,8). efficiency of that sample. The radionuclide used must be the
3.3.12 chemical quenching—a reduction in the scintillation same as that in the sample to be measured, the cocktail should
intensity (a significant interference with these test methods) be the same as the sample, the activity of the Internal Standard,
seen by the Photomultiplier Tubes (PMT, pmt) due to the and the Internal Standard must be of certified activity (13,16).
materials present in the scintillation solution that interfere with 3.3.25 modern carbon—explicitly, 0.95 times the specific
the processes leading to the production of light. The result is activity of SRM 4990b (the original oxalic acid radiocarbon
fewer photons counted and a lower efficiency (3,6,16). standard), normalized to d13C = −19 % (Currie, et al., 1989).
3.3.13 chi-square test—a statistical tool used in radioactive Functionally, the fraction of modern carbon equals 0.95 times
counting in order to compare the observed variations in repeat the concentration of 14C contemporaneous with 1950 wood
counts of a radioactive sample with the variation predicted by (that is, pre-atmospheric nuclear testing). To correct for the
statistical theory. This determines whether two different distri- post 1950 bomb 14C injection into the atmosphere (8), the
butions of photon measurements originate from the same fraction of modern carbon is multiplied by 0.93 (as of the year
photonic events. LSC instruments used in this measurement 2004).
should include this capability (13,16,26). 3.3.26 noise pulse—a spurious signal arising from the
3.3.14 cocktail—the solution in which samples are placed electronics and electrical supply of the instrument
for measurement in a LSC. Solvents and Scintillators (chemi- (13,16,20,28).
cals that absorbs decay energy transferred from the solvent and 3.3.27 phase contact—the degree of contact between two
emits light (photons) proportional in intensity to the decay phases of heterogeneous samples. In liquid scintillation count-
energy) (3,6,13,16). ing, better phase contact usually means higher counting effi-
3.3.15 decay (radioactive)—the spontaneous transforma- ciency (13,16).
tion of one nuclide into a different nuclide or into a different 3.3.28 photomultiplier tube (PMT, pmt)—the device in the
energy state of the same nuclide. The process results in a LSC that counts the photons of light simultaneously at two
decrease, with time, of the number of original radioactive separate detectors (28,31).
atoms in a sample, according to the half-life of the radionuclide
(7,13,16). 3.3.29 pulse—the electrical signal resulting when photons
are detected by the Photomultiplier tubes (13,16,17,31).
3.3.16 discriminator—an electronic circuit which distin-
guishes signal pulses according to their pulse height or energy; 3.3.30 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 (13,16,17,31). (13,16,17,31).
3.3.17 effıciency—the ratio of measured observations or 3.3.31 pulse index—the number of afterpulses following a
counts compared to the number of decay events which oc- detected coincidence pulse (used in three dimensional or pulse
curred during the measurement time; expressed as a percentage height discrimination) to compensate for the background of a
(13,16). liquid scintillation counter performing (13,17,28,31).
3.3.18 external standard—a radioactive source placed adja- 3.3.32 quenching—any material that interferes with the
cent to the liquid sample in to produce scintillations in the accurate conversion of decay energy to photons captured by the
sample for the purpose of monitoring the sample’s level of PMT of the LSC (1,3,6,13,14,16,19).
quenching. Required with Method (A) (13,16). 3.3.33 region—regions of interest, also called window
3.3.19 figure of merit—a term applied to a numerical value and/or channel in regard to liquid scintillation counters. Refers
used to characterize the performance of a system. In liquid to an energy level or subset specific to a particular isotope
scintillation counting, specific formulas have been derived for (3,13,17,20,28).

2
 D 6866 – 05
3.3.34 scintillation reagent—chemicals that absorbs decay 4.5 Although Methods A and C are less sensitive than that of
energy transferred from the solvent and emits light (photons) using AMS/IRMS, they have two distinct advantages: (1)
proportional in intensity to the decay energy (3,13,28). lower costs per evaluation, and (2) much higher instrument
3.3.35 solvent—in scintillation reagent, chemical(s) which availability worldwide. Benzene synthesis is the preferred
act as both a vehicle for dissolving the sample and scintillator method to be used when sample size is not an issue. Indeed,
and the location of the initial kinetic energy transfer from the LSC is the most widely used measurement for 14C determina-
decay products to the scintillator; that is, into excitation energy tion. Method B will be used primarily in extraordinary situa-
that can be converted by the scintillator into photons tions such as when the authenticities of the LSC radiocarbon
(3.13,16,28). results are in dispute, when sample size is greatly restricted or
3.3.36 standard count conditions (STDCT)—LSC condi- costly per mass of sample, or when the carbon content of the
tions under which reference standards and samples are sample is less than 10 % by weight.
counted. 4.6 The test methods described here directly discriminate
3.3.37 three dimensional spectrum analysis—the analysis of between product carbon resulting from contemporary carbon
the pulse energy distribution in function of energy, counts per input and that derived from fossil-based input. A measurement
energy, and pulse index. It allows for auto-optimization of a of a product’s 14C/12C content is determined relative to the
liquid scintillation analyzer allowing maximum performance. modern carbon-based oxalic acid radiocarbon Standard Refer-
Although different Manufacturers of LSC instruments call
ence Material (SRM) 4990c, (referred to as HOxII). It is
Three Dimensional Analysis by different names, the actual
compositionally related directly to the original oxalic acid
function is a necessary part of these test methods (13,16,17).
radiocarbon standard SRM 4990b (referred to as HOxI), and is
3.3.38 true beta event—an actual count which represents
denoted in terms of fM, that is, the sample’s fraction of modern
atomic decay rather than spurious interference (9,10).
carbon. (See Terminology, Section 3.)
3.3.39 flexible tube cracker—the apparatus in which the
sample tube (Break Seal Tube) is placed (4,5,9,10). 4.7 Reference standards, available to all laboratories prac-
3.3.40 break seal tube—the sample tube within which the ticing these test methods, must be used properly in order that
sample, copper oxide, and silver wire is placed. traceability to the primary carbon isotope standards are estab-
lished, and that stated uncertainties are valid. The primary
4. Significance and Use standards are SRM 4990c (oxalic acid) for 14C and RM 8544
4.1 Presidential (Executive) Orders 13101, 13123, 13134, (NBS 19 calcite) for 13C. These materials are available for
Public Laws (106-224, 107.117), AG ACT 2003 and other distribution in North America from The National Institute of
Legislative Actions all require Federal Agencies to develop Standards and Technology (NIST), and outside North America
procedures to identify, encourage and produce products de- from the International Atomic Energy Agency (IAEA), Vienna,
rived from biobased, renewable, sustainable and low environ- Austria.
mental impact resources so as to promote the Market Devel- 4.8 Acceptable SI unit deviations (tolerance) for the practice
opment Infrastructure necessary to induce greater use of such of these test methods is 65 % from the stated instructions
resources in commercial, non food, products. unless otherwise noted.
4.2 Method A utilizes Liquid Scintillation Counting (LSC)
radiocarbon (14C) techniques to quantify the biobased content 5. Safety
of a given product with maximum total error of 15 % count,
which is associated with sample preparation and actual count- 5.1 The specific safety and regulatory requirements associ-
ing. This test method is based on LSC analysis of CO2 ated with radioactivity, sample preparation, and instrument
cocktails after collecting the CO2 in a suitable absorbing operation are not addressed in these test methods. It is the
solution. responsibility of the user of these test methods to establish
4.3 Method B utilizes Accelerator Mass Spectrometry appropriate safety and health practices. It is also incumbent on
(AMS) and Isotope Ratio Mass Spectrometry (IRMS) tech- the user to conform to all the Federal and State regulatory
niques to quantify the biobased content of a given product with requirements, especially those that relate to the use of open
possible uncertainties of 1 to 2 % and 0.1 to 0.5 %, respec- radioactive source, in the performance of these test methods.
tively. Sample preparation methods are identical to Method A, Although 14C is one of the safest isotopes to work with, State
9.2–9.5. Method B diverges after 9.5 and rather than LSC and Federal regulations must be followed in the performance of
analysis the sample CO2 remains within the vacuum manifold these test methods.
and is distilled, quantified in a calibrated volume, transferred to 5.2 The use of glass and metal, in particular with closed
a quartz tube, torch sealed. Details are given in 12.7-12.10. The systems containing oxygen that are subjected to 700°C tem-
stored CO2 is then delivered to an AMS facility for final peratures pose their own safety concerns and care should be
processing and analysis. taken to protect the operators from implosion/explosion of the
4.4 Method C uses LSC techniques to quantify the biobased glass tube. Strong bases used for CO2 absorption, including
content of a product. However, whereas Method A uses LSC Carbosorb E+ which is also flammable, are particularly haz-
analysis of CO2 cocktails, Method C uses LSC analysis of ardous and instructions in Material Safety Data Sheets should
sample carbon that has been converted to benzene. This test be followed with special concern for eye protection.
method determines the biobased content of a sample with a Radioactive 14C compounds should be handled and disposed of
maximum total error of 63 % (absolute). in accordance with State and Federal Regulations.

3
 D 6866 – 05
5.3 In Method C, benzene is generated from the sample ~cpmb 2 cmpa!
E5 D (1)
carbon. Benzene is highly toxic and is an EPA-listed carcino-
gen. It must be handled accordingly, using all appropriate eye,
where:
skin, and respiratory protection. Samples must be handled and
E = counting efficiency,
disposed of in accordance with State and Federal regulations. cpma = standard counts of (STDCT) sample without added
Other hazardous chemicals are also used, and must be handled known activity,
appropriately (see Material Safety Data Sheets for proper cpmb = counts of (STDCT) sample plus added known
handling procedures). activity, and
D = dpm of the internal standard.
METHOD A Other counting interference concerns that must be addressed
as part of specific instrument calibration and normalization
6. Detailed Requirements include luminance, static electricity, random noise, temperature
NOTE 1—Acceptable tolerance levels of 65 % are standard to this and humidity variability.
method unless otherwise stated. 6.16 Alternate regions of interest parameters may be used
based upon testing of twenty, or more, 6 h counts of the same
6.1 Low Level Liquid Scintillation analyzers with active reference (STDCT) standard that record the raw data and
shielding. spectrum for KEV regions of interest 4 through 96. Optimal
6.2 Anticoincidence systems such as 2 and 3 Photomulti- energy windows counting should be determined by comparison
plier Tubes (Multidetector systems). of E2/bkg values to obtain the highest count efficiency and the
6.3 Coincidence circuits. lowest background and other interference. Counting efficiency
6.4 Software that includes thresholds, and statistics; Pulse of less that 60 % is unacceptable and can be improved by LSC
rise and shape discrimination, and three Dimensional Spectrum instrument optimization and sample/reagent compatibility or
Analysis. shielding improvements.
6.5 Use of External and Internal Standards. 6.17 All samples will be allowed to equilibrate for a
6.6 Optimized counting regions to provide very low back- minimum of 8 h prior to counting and will be inspected for
ground counts while maintaining counting efficiency greater phase separation after the period of equilibration and prior to
than 60 % of samples 0.7 to 1.5 g in clean, 20-mL Low counting.
Potassium glass count vials. 6.18 Samples will be counted for a minimum of 20 h with
6.7 No single Liquid Scintillation Counter is specified for region of interest integrals (RIO) channels including RIO
this method. However, minimum counting efficiency and energy levels of 10 to 82 in 120 min subsets with complete
control of background interference is specified. Like all ana- spectra saved to disk as well as raw data for later statistical
lytical instruments, LS counters require study as to their analysis and inclusion with final report.
specific components and counting optimization. 6.19 Prior to commercial testing, laboratories that intend to
6.8 Standardization of sample preparation is required. implement this method must participate in an inter-laboratory
6.9 External and internal standards must be used in LSC comparison study to in order to assess between laboratory
operation. reproducibility.
6.10 Standardization and optimization of 20-mL sample
vials, which must be of clean, low potassium glass with PTFE 7. Apparatus and Reagents
insert tops. Inspect scintillation vials for contaminants such as
NOTE 3—Certain commercial equipment, instruments or materials are
dirt, oils, or residues. Do not use the vials if they do not appear identified to specify adequately the experimental procedure. Such identi-
to be clean. fication does not imply recommendation or endorsement by the ASTM or
NOTE 2—Plastic vials should not be used for this method. by NIST, nor does it imply that the materials or equipment are necessarily
the best available for the purpose. A great deal of effort has been expended
6.11 Optimization of Scintillation Cocktail, CO2 trap re- to optimize reagents. Suggestions are provided for ease of practice of the
agents, and additives such as emulsifiers, surfactants, alcohols, method.
and sample material is required. 7.1 A key to the ease of application of Method (A) is the
6.12 Optimization of reagents shall include sample to re- selection of cocktail components. The interaction and compat-
agent volume, scintillator to CO2 trap reagent and additive ibility of these chemicals can produce one of the greatest
volumes and compatibility of all reagents. sources of interference with the method. One possible combi-
6.13 Quench curves and counting efficiency and back- nation for Method (A) = 12 mL of Ultima Gold Scintillation
ground optimization should be performed using a reference Reagent + 6 mL of Carbosorb CO2 trapping reagent (that
standard based on comparison to NIST oxalic acid reference contains the trapped CO2 resulting from combustion of the
standards and the same reagents and counting parameters as the sample) + 2 mL of high quality (spectrometer grade) methanol.
samples. Although other combinations are allowed, the combination
6.14 Counting efficiency of the sample shall be determined used must produce an efficiency of greater than 75 % using the
by adding to a vial a known activity of the same radionuclide Reference Standard from NIST. Otherwise the combination
and computing the increase of the sample cpm. should not be used. Commercial oxidizers are available, and
6.15 The internal standard technique for computing count- can be adapted to produce a carbon dioxide sample for carbon
ing efficiency should be calculated by the equation: dating. Such a commercial oxidizer may be used to prepare the

4
 D 6866 – 05
samples for LSC analysis in Method (A) if the adaptations can 8.3 The weighed sample shall then be transferred into an
produce a sample with the following minimum requirements: appropriately sized quartz tube, typically 6 mm OD/4 mm ID.
7.1.1 Temperature of oxidation and oxidation time are 8.4 The sample, thus configured shall then be adapted to a
sufficient to produce carbon recovery as CO2 in CO2 trap vacuum manifold for evacuation of ambient air to a pressure
reagent at a minimum of 98 %. 101.3 Pa or less. If the material is known to be volatile or
7.1.2 LSC Count Efficiency of the sample is greater than contains volatile components, the sample material within the
60 %. tube shall be frozen with liquid nitrogen to –196°C prior to
7.2 LSC Apparatus: evacuation. The evacuated tube shall be torch sealed then
7.2.1 A vacuum manifold system with capabilities for air combusted in a temperature controlled furnace at 400°C for 2
and non-condensable gas evacuation, sample introduction, to 4 h. Otherwise the material will be torch sealed at one end
water distillation, cryogenic gas transfer, and temperature and and furnace-baked at 900°C for $2 h.
pressure monitoring. 8.5 After combustion, the quartz sample tube shall be scored
7.2.2 Manifold with tubing that is composed of clean to facilitate a clean break within a flexible hose portion of a
stainless steel and/or glass. “tube cracker” assembly adapted to the manifold. One example
7.2.3 Vacuum pump(s) capable of achieving a vacuum of configuration of a tube cracker is shown in the photo in the
101 Pa or less within the vacuum region. Appendixes to these test methods. The materials are composed
7.2.4 Three-way valve adapted to the manifold at one valve of stainless steel. Compression fittings with appropriate welds
to vacuum, another to cryogenic liquid Nitrogen, and the other are used to assemble the individual parts. This and alternative
valve position closed to all but the sample. assemblies are also identified in the References section of these
7.2.5 A second three-way valve adapted to the manifold at test methods (4,5,9,10).
one valve to cryogenic liquid Nitrogen, to a valve connected to 8.6 With the manifold closed to the vacuum pump, the
a reservoir of liquid CO2 trap reagent, and the other valve quartz tubing is cracked, the sample CO2 is liberated and
position closed to all but the sample. immediately cryogenically (with liquid nitrogen) transferred to
7.2.6 A sample bulb adapted to the manifold. a sample collection bulb also attached to a separate port on the
7.2.7 Clean quartz tubing for sample combustion and sub- manifold.
sequent gas transfer, quantification and storage. 8.7 A three-way valve (or electronic equivalent) attached to
7.2.8 A hydrogen/oxygen torch or other heating device the sample bulb will be open to allow the CO2 to enter the
and/or gas for sealing quartz tubing. sample bulb. It will be then turned to allow the addition of 6
7.2.9 Flexible Tube Cracker. mL of CO2 trapping reagent. The three-way valve is then
7.2.10 Break Seal Tube. closed and the sample is allowed to remain undisturbed for a
7.2.11 Liquid Scintillation Analyzer as described in Section minimum of 1 h. The sample should then be further processed
6. within 3 h.
7.2.12 Clean scintillation vials, 20-mL volume, with PTFE- 8.8 After 1 to 3 h, the sample bulb is removed from the
lined screw caps. manifold. The trapping reagent is then transferred to a 20 mL
7.2.13 Long thin pipettes for transfer of the sample from the glass Scintillation vial.
sample bulb to the scintillation vial. 8.9 To the sample vial is added 2 mL of methanol and 12
7.3 LSC Reagents: mL of compatible scintillation reagent.
7.3.1 A stoichiometric excess oxygen for sample combus- 8.10 A PTFE-lined cap is screwed tight on the vial and the
tion; introduced into sample tube as either a pure gas or as solid vial is inverted 10 times.
copper (II) oxide. 8.11 All samples will then be allowed to equilibrate for a
7.3.2 A stoichiometric excess of silver, nominally 30 mg, minimum of 8 h prior to counting and will be inspected for
introduced into sample tube for the removal of halogenated phase separation after the period of equilibration and prior to
species. counting. Samples may be counted at any time after the 8 h as
7.3.3 A −76°C slurry mixture of dry ice (frozen CO2) and long as phase separation has not taken place.
alcohol distillation and removal of sample water. 8.12 The 14C content shall be determined in a Liquid
7.3.4 Liquid nitrogen. Scintillation Counter with optimization of the instrument as
7.3.5 Scintillation reagent. described in the References section.
7.3.6 CO2 trapping reagent. 8.13 Samples will be maintained for recounting within the
7.3.7 Methanol, spectrometry grade. laboratory for a minimum of 180 days.
8.14 The sample will then be disposed of in accordance with
8. Sample Preparation and Analysis State and Federal Regulations.
8.1 Tolerance of 65 % is to be assumed unless otherwise
stated. 9. Interpretation
8.2 Based on the stoichiometry of the product material, 9.1 The counts shall be compared, directly or through
sufficient sample mass shall be weighed such that 0.500 to secondary standards, to the 14C oxalic acid SRM 4990c, with
1.000 g of carbon are quantitatively recovered as CO2. Typi- stated uncertainties. Significantly lower 14C counts indicate the
cally 2 mm OD/1 mm ID quartz tubing is sufficient, however presence of 14C-depleted carbon. Zero percent 14C, when com-
any tubing configuration needed to accommodate large sample pared to the standard, signifies the entire lack of 14C atoms in
volumes is acceptable. a material thus indicating a fossil (for example, petroleum

5
 D 6866 – 05
based) carbon source. One hundred percent 14C, after correc- sufficient, however any tubing configuration needed to accom-
tion for the post-1950 bomb injection of 14C into the atmo- modate large sample volumes is acceptable.
sphere, likewise signifies an entirely modern carbon source. 12.3 The weighed sample shall then be transferred into an
The percent modern carbon can be slightly greater than 100 % appropriately sized quartz tube, typically 6 mm OD/4 mm ID.
due to the continuing, but diminishing, effects of the 1950s 12.4 The sample, thus configured shall then be adapted to a
nuclear testing programs. Because all sample 14C activities are vacuum manifold for evacuation of ambient air to a pressure
referenced to a “pre-bomb” standard, all percent modern 101 Pa or less.
carbon values must be multiplied by 0.93 to correct for the 12.5 If the material is known to be volatile or contains
bomb carbon and to subsequently obtain the true biobased volatile components, the sample material within the tube shall
content of the sample. be frozen with liquid nitrogen to –196°C prior to evacuation.
The evacuated tube shall be torch sealed then combusted in a
METHOD B temperature controlled furnace at 900°C for 2 to 4 h.
12.6 After combustion, the quartz sample tube shall be
10. Apparatus and Reagents scored to facilitate a clean break within a flexible hose portion
10.1 AMS and IRMS Apparatus: of a “tube cracker” assembly adapted to the manifold. One
10.1.1 A vacuum manifold system for with capabilities for example configuration of a tube cracker is shown in the photo
air and non-condensable gas evacuation, sample introduction, below. The materials are composed of stainless steel. Compres-
water distillation, cryogenic gas transfer, and temperature and sion fittings with appropriate welds are used to assemble the
pressure monitoring. The following equipment is required: individual parts. This and alternative assemblies are given in
10.1.2 Manifold tubing that is composed of clean stainless the References section (4,5,9,10).
steel and/or glass. 12.7 With the manifold closed to the vacuum pump, the
10.1.3 Vacuum pump(s) capable of achieving a vacuum of quartz tubing is cracked, the sample CO2 is liberated and
101 Pa or less within the vacuum region. immediately cryogenically (with liquid nitrogen) transferred to
10.1.4 Calibrated pressure transducers with coupled or in- a sample collection bulb attached to a separate port on the
tegrated signal response controllers. manifold.
10.1.5 A calibrated sample collection volume with associ- 12.8 The contents of the sample collection bulb shall be
ated temperature readout. distilled to remove residual water using a dry ice/alcohol slurry
10.1.6 Clean quartz tubing for sample combustion and maintained at ca. −76°C. Simultaneously the sample CO2 gas
subsequent gas transfer, quantification and storage. is released and immediately condensed in a calibrated volume.
10.1.7 A hydrogen/oxygen torch or other heating device 12.9 The calibrated volume is then closed and the CO2 shall
and/or gas for sealing quartz tubing. equilibrate to room temperature.
12.10 Recovery shall be determined using the ideal gas law
11. AMS and IRMS Reagents relationship.
12.11 The sample shall be transferred to a borosilicate break
11.1 A stoichiometric excess oxygen for sample combus- seal tube for storage and delivery to an AMS facility for
tion; introduced into sample tube as either a pure gas or as solid analysis of 14C/12C and 13C/12C isotopic ratios.
copper (II) oxide.
11.2 A stoichiometric excess of silver, nominally 30 mg, 13. Analysis, Interpretation, and Report
introduced into sample tube for the removal of halogenated 13.1 14C/12C and 13C/12C isotopic ratios are counted (14C)
species. and measured 13C/12C using accelerator mass spectrometry.
11.3 A −76°C slurry mixture of dry ice (frozen CO2) and The isotopic ratios of 14C/12C and 13C/12C are determined
alcohol distillation and removal of sample water. relative to the appropriate primary reference material, that is,
11.4 Liquid nitrogen. SRM 4990c and RM 8544, for 14C and 13C, respectively. Zero
percent 14C represents the entire lack of 14C atoms in a material
12. Sample Preparation thus indicating a fossil (for example, petroleum based) carbon
12.1 Method B is a commonly used procedure to quantita- source. One hundred percent 14C, after correction for the
tively combust the carbon fraction within product matrices of post-1950 bomb injection of 14C into the atmosphere, likewise
varying degrees of complexity. The procedure described here indicates an entirely modern carbon source. The percent
for Method B is recommended based on its affordability and modern carbon can be slightly greater than 100 % due to the
extensive worldwide use Nevertheless, laboratories with alter- continuing, but diminishing, effects of the 1950s nuclear
native instrumentation such as continuous flow interfaces and testing programs. Because all sample 14C activities are refer-
associated CO2 trapping capabilities are equally suitable pro- enced to a “pre-bomb” standard, all percent modern carbon
vided that the recovery of CO2 is quantitative, 100 6 5 %. values must be multiplied by 0.93 to correct for the bomb
12.2 Based on the stoichiometry of the product material, carbon and to subsequently obtain the true biobased content of
sufficient sample mass shall be weighed such that 1-10 mg of the sample. References for reporting carbon isotopic ratio data
carbon is quantitatively recovered as CO2. Weighed sample are given in Refs (26,2) for 14C and 13C, respectively.
material shall be contained within a pre-cleaned quartz sample 13.2 All percent modern carbon (pMC) values obtained
container, furnace-baked at 900°C for $2 h, and torch sealed at from the radiocarbon analyses must be corrected for isotopic
one end. Typically 2 mm OD/1 mm ID quartz tubing is fractionation (27) using stable isotope data (13C/12C ratios)

6
 D 6866 – 05
obtained on CO2 derived from combustion of the sample. Do spectrum for keV regions of interest 4 through 96. Optimal
not determine 13C/12C ratios on the raw product material itself, counting conditions should be established by maximizing the
since that approach can lead to erroneous results in some cases. Figure of Merit (E2/bkg) values to obtain the highest count
efficiency and the lowest background and other interference.
METHOD C Counting efficiency of less that 60 % is unacceptable and can
14. Detailed Requirements be improved by LSC instrument optimization and sample/
reagent compatibility or shielding improvements.
NOTE 4—Acceptable tolerance levels of 65 % are standard to this 14.14 Samples will be equilibrated with reference standards
method unless otherwise stated.
under identical conditions of time and temperature.
14.1 Low level liquid scintillation analyzers with active 14.15 Samples will be counted for a minimum of 10 h with
shielding that can produce consistent background counts of less region of interest (ROI) channels including ROI energy levels
than 5 dpm. of 0-155 keV such that E2/B is 1000 or higher in 20 to 120-min
14.2 Anticoincidence systems such as two and three photo- subsets with raw data saved to disk for later statistical analysis
multiplier tubes (multidetector systems). and documentation of stable counting conditions.
14.3 Coincidence circuits. 14.16 Before commercial testing, laboratories that intend to
14.4 Software and hardware that include thresholds and implement this method must participate in an interlaboratory
statistics, pulse rise and shape discrimination, and three- comparison study to assess between laboratory reproducibility.
dimensional spectrum analysis.
14.5 Use of external and internal standards must be used in 15. Apparatus and Reagents
LSC operation.
15.1 Benzene Synthesis Apparatus
14.6 Optimized counting regions to provide very low back-
15.1.1 A benzene synthesis unit will be required to convert
ground counts while maintaining counting efficiency greater
sample carbon to benzene. These units are commercially
than 60 % of samples 0.7 to 1.5 g in clean, 3-mL, 7-mL or
available, but can also be home-made if desired. Examples of
20-mL low potassium glass counting vials. Alternatively, clean
benzene synthesis units are discussed in (11) and (29).
PTFE or quartz counting vials may be used in this method.
15.2 LSC Apparatus
14.7 No single LSC is specified for this method. However,
15.2.1 Liquid scintillation analyzer as described in Section
minimum counting efficiency and control of background inter-
14.
ference is specified. Like all analytical instruments, LS
15.2.2 Clean scintillation vials with a volume of 3 mL, 7
counters require study as to their specific components and
mL, or 20 mL.
counting optimization.
15.3 LSC and Benzene Synthesis Reagents
14.8 Standardization of sample preparation is required.
15.3.1 High purity oxygen for converting sample carbon to
14.9 Standardization and optimization of clean sample vi-
CO2. Alternatively, technical grade oxygen can be used if
als, which must be made of either PTFE, quartz, or low-
scrubbed with a suitable material such as Ascarite.
potassium glass with PTFE tops. Sample vials may be either
15.3.2 High purity nitrogen for combining with the oxygen
3-mL, 7-mL or 20-mL in volume. Plastic vials must not be used
when combusting highly volatile samples. Alternatively, tech-
for this method.
nical grade nitrogen can be used is scrubbed with a suitable
14.10 Counting efficiency and background optimization
material such as Ascarite.
should be performed using a suitable reference standard (for
example, NIST oxalic acid or ANU sucrose) using the same 15.3.3 Cupric oxide wire for conversion of CO to CO2 when
reagents and counting parameters as the samples. combusting highly volatile samples with oxygen/nitrogen
14.11 Counting efficiency (E) shall be determined by divid- blends.
ing the measured cpm by the known dpm, and multiplying this 15.3.4 Reagent grade powdered lithium or lithium rod (each
by 100 to obtain the counting efficiency as a percentage. For packed in argon) for converting CO2 to lithium carbide
example, for the Oxalic Acid I standard, E = (cpm/g Oxalic (Li2C2).
Acid/ 14.27 dpm/g) 3 100, where E = counting efficiency in 15.3.5 Reagent grade potassium chromate (in sulfuric acid)
%, cpm/g Oxalic Acid is the net activity per gram measured for or phosphoric acid for purifying acetylene gas.
the oxalic acid after subtracting background, and 14.27 dpm/g 15.3.6 Suitable catalyst material such as a Si2O3/Al2O3
is the absolute value of the NIST “Ox I” reference standard. substrate activated with either chromium (as Cr2O3) or vana-
The NIST “Ox II” standard (SRM 4990C) has a slightly dium (as V2O5) for converting acetylene gas to benzene (22).
different 14C activity level. ANU sucrose (NIST SRM 8542) 15.3.7 Scintillation reagent.
can be used as a suitable standard in place of oxalic acid. 15.3.8 De-ionized or distilled water for hydrolysis of Li2C2
14.12 Counting interference concerns that must be ad- to acetylene gas.
dressed as part of specific instrument calibration and normal-
ization include luminance, chemical or color quench, static 16. Sample Preparation and Analysis
electricity, random noise, temperature, and humidity variability 16.1 Tolerance of 65 % is to be assumed unless otherwise
(12). stated.
14.13 Alternate regions of interest parameters may be used 16.2 Standard procedures are to be employed for the con-
based upon testing of 20, or more, 6-h counts of the same version of original sample material to benzene using the liquid
reference (STDCT) standard that record the raw data and scintillation dating technique (11).

7
 D 6866 – 05
16.3 Based on the stoichiometry of the product material, A recommended scintillator is butyl-PBD or PPO/POPOP
sufficient sample mass shall be weighed such that quantitative dissolved in toluene or equivalent (12) and (15). Alternatively,
recovery of the carbon would theoretically yield 1.00 to 4.00 g some scintillators (including butyl-PBD) can be added to the
of carbon for conversion to benzene. benzene as a solid with good results.
16.4 The carbon within each sample shall first be combusted 16.15 Standard methods consist of counting a cocktail
to CO2 by placing the sample in a closed system which is containing sample benzene plus a scintillation solution. For
purged or evacuated of air. example, a cocktail might contain 4 mL sample benzene plus
16.5 The system is then purged several times with pure 0.5 mL scintillation solution. In this example, if 4 mL of
nitrogen. After verifying the integrity of the closed system, the sample benzene is not available, reagent grade (99.999% pure)
sample is bathed in 100 % oxygen (non-volatile samples) or a thiophene-free benzene can be added to bring the sample
mixture of nitrogen and oxygen (volatile samples) and ignited. volume to 4 mL. Larger or smaller volumes may be utilized
Samples ignited using a nitrogen/oxygen mix must pass depending upon the configuration of the specific laboratories
through a cupric oxide furnace at 850°C to avoid carbon loss to counting protocols.
CO. The generated sample CO2 is collected using liquid 16.16 Scintillation counters are to be monitored for back-
nitrogen cold traps. If desired, the CO2 can be passed through ground and stability with traceable documentation.
a series of chemical traps to remove various contaminants prior 16.17 Should anomalies appear during sample counting, the
to cryogenic collection of the CO2 (11). benzene is to be re-measured in another counter to verify the
16.6 As an alternative combustion approach for volatile activity, or the sample must be completely re-analyzed.
materials, the samples can be combusted in a Parr bomb that is 16.18 Traceable quench detection should be performed on
pressurized with oxygen to 300-400 psi. The CO2 generated in each sample to ensure benzene purity. In the event the sample
the Parr bomb is subsequently released to a dry ice trap for is substantially quenched, the data should be discarded and the
moisture removal, followed by a liquid nitrogen cold trap for sample should be re-analyzed.
CO2 collection. 16.19 Measurements are to be made on an interval basis
16.7 The collected CO2 is reacted with a stoichiometric (usually 50 or 100 minutes) to allow statistical analysis of the
excess (3:1 lithium:carbon ratio) of molten lithium which has measurement.
been preheated to 700°C. Li2C2 is produced by slowly bleeding 16.20 Prior to removing the sample from the counter,
the CO2 onto the molten lithium in a stainless steel vessel (or stability is to be verified and the data scrutinized for anomalies.
equivalent) while under a vacuum of #135 mPa. If the distribution does not closely follow Gaussian statistics,
16.8 The Li2C2 is heated to about 900°C and placed under the sample should be transferred and counted in another
vacuum for 15-30 minutes to remove any unreacted gases and counter for verification, or the sample should be completely
to complete the Li2C2 synthesis reactions (26). re-analyzed.
16.9 The Li2C2 is cooled to room temperature and gently 16.21 Counting should be performed as needed to obtain a
hydrolyzed with distilled or de-ionized water to generate precision of 2 % or better.
acetylene gas (C2H2) by applying the water in a drop-wise 16.22 Calculation of the data should be performed only after
fashion to the carbide. The evolved acetylene is dried by cross-checking all transcribed numbers, synthesis records,
passing it through dry ice traps, and the dried acetylene in cocktail preparation, counting data, and counting analysis.
subsequently collected in liquid nitrogen traps. 16.23 Any unused sample material shall be maintained at
16.10 The acetylene gas is purified by passing it through a the laboratory for potential re-analysis for a minimum of 180
phosphoric acid or potassium chromate (in sulfuric acid) trap to days. The sample will then be disposed of in accordance with
remove trace impurities, and by using dry ice traps to remove state and federal regulations.
water. 16.24 Because of problems in storing benzene over ex-
16.11 The C2H2 gas is catalyzed to benzene (C6H6) by tended periods of time, it may be necessary to re-distill (to
bleeding the acetylene onto a chromium catalyst which has remove scintillant) and re-weigh the benzene if re-analysis is
been preheated to $90°C, or onto a vanadium catalyst (the desired at a later date. Alternatively, a fresh portion of the
later activates at ambient temperature). In the former case, the biobased product can be processed to obtain a fresh benzene
reaction is cooled with a water jacket to avoid decomposition sample.
from excessive heat generated during the exothermic reaction. NOTE 5—The benzene derived from the sample carbon is toxic and is a
16.12 The benzene is thermally evolved from the catalyst at known carcinogen. Special handling and disposal procedures will be
70-110°C and then collected under vacuum at roughly -78°C. required.
The benzene is then frozen until it is counted. Radon can be
removed by pumping on the benzene while it is at dry ice 17. Interpretation
temperatures. 17.1 The counts shall be compared, directly or through
16.13 The 14C content shall be determined in a LSC with secondary standards, to the 14C oxalic acid SRM 4990c (or
optimization of the instrument as described in Section 14. other suitable standard), with stated uncertainties. Significantly
Either single vial counting or “chain” counting is acceptable. lower 14C counts indicate the presence of 14C-depleted carbon.
16.14 Radiocarbon activity in the sample is to be deter- The lack of any 14C counts in a material indicates a fossil (for
mined by “benzene cocktail” analysis, consisting of a scintil- example, petroleum based) carbon source. A sample that has
lator plus sample benzene, in constant volume and proportion. the same 14C activity level (after correction for the post-1950

8
 D 6866 – 05
bomb injection of 14C into the atmosphere) as the oxalic acid “pre-bomb” standard, and because nearly all new biobased
standard is 100 % biobased and signifies an entirely modern products are produced in a post-bomb environment, all pMC
carbon source. The inherent assumption is that all of the values (after correction for isotopic fractionation) must be
organic components within the analyzed material are either multiplied by 0.93 (as of the writing of this standard) to better
fossil or present day in origin. reflect the true biobased content of the sample.
17.2 All percent modern carbon (pMC) values obtained
from the radiocarbon analyses must be corrected for isotopic 18. Precision and Bias
fractionation (27) after performing stable carbon isotope analy- 18.1 The precision and bias of Method A will be determined
ses (13C/12C ratios). The stable isotope analyses must be by Round Robin testing between laboratories practicing the
performed on a portion of the CO2 derived from the combus- method and will be available on or before December 2007.
tion of the sample. 18.2 The precision and bias of Method B from any reporting
17.3 The percent modern carbon can be greater than 100 % laboratory will be deemed acceptable if it can be shown that the
because of the continuing but diminishing effects of the 1950s data are traceable to the primary standards and within the
nuclear testing programs, which resulted in a considerable uncertainties stated in 4.3. If deviations from these criterions
enrichment of 14C in the atmosphere. The decrease in 14C from are pervasive a Round Robin testing will be implemented and
the bomb testing programs has been nonlinear. Although it will be available on or before December 2007.
continues to decrease by a small amount each year, the
current 14C activity in the atmosphere has not reached the 1950 19. Keywords
level of 13.56 dpm per gram carbon that is defined as 100 19.1 biobased;14C (carbon-14); carbon dating; new carbon;
pMC. Because all sample 14C activities are referenced to a old carbon

9
 D 6866 – 05

APPENDIX

(Nonmandatory Information)

X1. FIGURES

FIG. X1.1 Example of a Gas Transfer Manifold

10
 D 6866 – 05

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

11
 D 6866 – 05

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

12
 D 6866 – 05
REFERENCES

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

13
 D 6866 – 05
SUMMARY OF CHANGES

Committee D20 has identified the location of selected changes to this standard since the last issue,
D 6866 - 04a, that may impact the use of this standard. (March 1, 2005)

(1) Corrected errors and improved clarity throughout.

(2) Added requirements to ensure that all labs use the same
reporting procedure.

Committee D20 has identified the location of selected changes to this standard since the last issue,
D 6866 - 04, that may impact the use of this standard. (July 1, 2004)

(1) Revised standard to incorporate Test Method C which

begins in Section 14.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or [email protected] (e-mail); or through the ASTM website
(www.astm.org).

14