ASTM-D6866 › Standard Test Methods for Determining the Biobased Content of Solid, Liquid, and Gaseous Samples Using Radiocarbon Analysis
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1.1 This standard is a test method that teaches how to experimentally measure biobased carbon content of solids, liquids, and gaseous samples using radiocarbon analysis. These test methods do not address environmental impact, product performance and functionality, determination of geographical origin, or assignment of required amounts of biobased carbon necessary for compliance with federal laws.
1.2 These test methods are applicable to any product containing carbon-based components that can be combusted in the presence of oxygen to produce carbon dioxide (CO2) gas. The overall analytical method is also applicable to gaseous samples, including flue gases from electrical utility boilers and waste incinerators.
1.3 These test methods make no attempt to teach the basic principles of the instrumentation used although minimum requirements for instrument selection are referenced in the References section. However, the preparation of samples for the above test methods is described. No details of instrument operation are included here. These are best obtained from the manufacturer of the specific instrument in use.
1.4 Limitation—This standard is applicable to laboratories working without exposure to artificial carbon-14 (14C). Artificial 14C is routinely used in biomedical studies by both liquid scintillation counter (LSC) and accelerator mass spectrometry (AMS) laboratories and can exist within the laboratory at levels 1,000 times or more than 100 % biobased materials and 100,000 times more than 1% biobased materials. Once in the laboratory, artificial 14C can become undetectably ubiquitous on door knobs, pens, desk tops, and other surfaces but which may randomly contaminate an unknown sample producing inaccurately high biobased results. Despite vigorous attempts to clean up contaminating artificial 14C from a laboratory, isolation has proven to be the only successful method of avoidance. Completely separate chemical laboratories and extreme measures for detection validation are required from laboratories exposed to artificial 14C. Accepted requirements are:
(1) disclosure to clients that the laboratory(s) working with their products and materials also works with artificial 14C
(2) chemical laboratories in separate buildings for the handling of artificial 14C and biobased samples
(3) separate personnel who do not enter the buildings of the other
(4) no sharing of common areas such as lunch rooms and offices
(5) no sharing of supplies or chemicals between the two
(6) quasi-simultaneous quality assurance measurements within the detector validating the absence of contamination within the detector itself. (, , and )
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
Note 1: ISO 16620-2 is equivalent to this standard.
1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Significance and Use
4.1 This testing method provides accurate biobased/biogenic carbon content results to materials whose carbon source was directly in equilibrium with CO2 in the atmosphere at the time of cessation of respiration or metabolism, such as the harvesting of a crop or grass living its natural life in a field. Special considerations are needed to apply the testing method to materials originating from within artificial environments. Application of these testing methods to materials derived from CO2 uptake within artificial environments is beyond the present scope of this standard.
4.2 Method B utilizes AMS along with Isotope Ratio Mass Spectrometry (IRMS) techniques to quantify the biobased content of a given product. Instrumental error can be within 0.1-0.5 % (1 relative standard deviation (RSD)), but controlled studies identify an inter-laboratory total uncertainty up to ±3 % (absolute). This error is exclusive of indeterminate sources of error in the origin of the biobased content (see Section 22 on precision and bias).
4.3 Method C uses LSC techniques to quantify the biobased content of a product using sample carbon that has been converted to benzene. This test method determines the biobased content of a sample with a maximum total error of ±3 % (absolute), as does Method B.
4.4 The test methods described here directly discriminate between product carbon resulting from contemporary carbon input and that derived from fossil-based input. A measurement of a product’s 14C/12C or 14C/13C content is determined relative to a carbon based modern reference material accepted by the radiocarbon dating community such as NIST Standard Reference Material (SRM) 4990C, (referred to as OXII or HOxII). It is compositionally related directly to the original oxalic acid radiocarbon standard SRM 4990B (referred to as OXI or HOxI), and is denoted in terms of fM, that is, the sample’s fraction of modern carbon. (See Terminology, Section .)
4.5 Reference standards, available to all laboratories practicing these test methods, must be used properly in order that traceability to the primary carbon isotope standards are established, and that stated uncertainties are valid. The primary standards are SRM 4990C (oxalic acid) for 14C and RM 8544 (NBS 19 calcite) for 13C. These materials are available for distribution in North America from the National Institute of Standards and Technology (NIST), and outside North America from the International Atomic Energy Agency (IAEA), Vienna, Austria.
4.6 Acceptable SI unit deviations (tolerance) for the practice of these test methods is ±5 % from the stated instructions unless otherwise noted.
accelerator mass spectrometry; biobased; biogenic; bomb carbon; 14C (carbon-14); carbon dating; isotope ratio mass spectrometry; liquid scintillation counting; new carbon; old carbon; percent modern carbon;
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Feb. 1, 2020