Bio-based products - Determination of the bio based carbon content of products using the radiocarbon method

CEN/TS 16640 specifies a method for the determination of the bio-based carbon content in products, based on the 14C content measurement. It also specifies three test methods to be used for the determination of the 14C content from which the biobased carbon content is calculated: - Method A: Liquid scintillation-counter method (LSC); - Method B: Beta-ionization (BI); - Method C: Accelerator mass spectrometry (AMS). The bio-based carbon content is expressed by a fraction of sample mass, as a fraction of the total carbon content or as a fraction of the total organic carbon content. This calculation method is applicable to any product containing organic carbon, including biocomposites.

Biobasierte Produkte - Bestimmung des biobasierten Kohlenstoffanteils von Produkten mittels Radiocarbonmethode

Diese Technische Spezifikation legt ein Verfahren zur Bestimmung des Gehalts an biobasiertem Kohlenstoff in Produkten auf der Grundlage der Messung des 14C-Gehalts fest.
Es werden auch drei Prüfverfahren festgelegt, die zur Bestimmung des 14C-Gehalts anzuwenden sind, aus dem der biobasierte Kohlenstoffgehalt berechnet wird:
 Verfahren A: Flüssigszintillationszählverfahren (LSC);
 Verfahren B: Beta-Ionisation (BI);
 Verfahren C: Beschleuniger-Massenspektrometrie (AMS).
Der biobasierte Kohlenstoffgehalt wird als Anteil der Masse der Probe angegeben, als Anteil des gesamten Gehalts an Kohlenstoff oder als Anteil des Gehaltes an organischem Kohlenstoff.
Dieses Berechnungsverfahren ist auf alle Produkte anwendbar, die organischen Kohlenstoff enthalten, einschließlich Bioverbundwerkstoffen.
ANMERKUNG Diese Technische Spezifikation bietet kein Verfahren für die Berechnung des Biomassegehalts einer Probe.

Produits biosourcés - Détermination de la teneur en carbone biosourcé des produits par la méthode du carbone radioactif

La présente Spécification technique spécifie une méthode permettant de déterminer la teneur en carbone biosourcé dans des produits à partir du mesurage de la teneur en 14C.
Elle spécifie également trois méthodes d'essai à utiliser pour déterminer la teneur en 14C, à partir de laquelle la teneur en carbone biosourcé est calculée :
-   Méthode A : compteur à scintillation liquide (CSL) ;
-   Méthode B : ionisation bêta (IB) ;
-   Méthode C : spectrométrie de masse par accélérateur (SMA).
La teneur en carbone biosourcé est exprimée en fraction de masse d'échantillon, en fraction de la teneur en carbone total ou en fraction de la teneur en carbone organique total.
Cette méthode de calcul est applicable à tout produit contenant du carbone organique, y compris les biocomposites.
NOTE   La présente Spécification technique ne fournit pas la méthodologie permettant de calculer la teneur en biomasse d'un échantillon.

Bioizdelki - Ugotavljanje deleža bioogljika v izdelkih z radioogljično metodo

Standard CEN/TS 16640 določa metodo za ugotavljanje deleža bioogljika v izdelkih na podlagi meritve deleža 14C. Prav tako določa tri preskusne metode za ugotavljanje deleža 14C, na podlagi katere se izračuna delež bioogljika: – metoda A: metoda števca s tekočinskim scintilatorjem (LSC); – metoda B: beta ionizacija (BI); – metoda C: pospeševalna masna spektrometrija (AMS). Delež bioogljika se izrazi z deležem mase vzorca kot delež skupnega deleža ogljika ali kot delež skupnega deleža organskega ogljika. Ta metoda izračuna se uporablja za vse izdelke, ki vsebujejo organski ogljik, vključno z biokompoziti.

General Information

Status
Withdrawn
Publication Date
31-Mar-2014
Withdrawal Date
07-May-2017
Technical Committee
Current Stage
9900 - Withdrawal (Adopted Project)
Start Date
03-May-2017
Due Date
26-May-2017
Completion Date
08-May-2017

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SLOVENSKI STANDARD
SIST-TS CEN/TS 16640:2014
01-maj-2014
%LRL]GHONL8JRWDYOMDQMHGHOHåDELRRJOMLNDYL]GHONLK]UDGLRRJOMLþQRPHWRGR
Bio-based products - Determination of the bio based carbon content of products using
the radiocarbon method
Biobasierte Produkte - Bestimmung des biobasierten Kohlenstoffanteils von Produkten
mittels Radiocarbonmethode
Produits biosourcés - Détermination de la teneur en carbone biosourcé des produits par
la méthode du carbone radioactif
Ta slovenski standard je istoveten z: CEN/TS 16640:2014
ICS:
13.020.60 Življenjski ciklusi izdelkov Product life-cycles
71.040.40 Kemijska analiza Chemical analysis
SIST-TS CEN/TS 16640:2014 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 16640:2014

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SIST-TS CEN/TS 16640:2014

TECHNICAL SPECIFICATION
CEN/TS 16640

SPÉCIFICATION TECHNIQUE

TECHNISCHE SPEZIFIKATION
March 2014
ICS 13.020.60; 71.040.40; 83.040.01
English Version
Bio-based products - Determination of the bio based carbon
content of products using the radiocarbon method
Produits biosourcés - Détermination de la teneur en Biobasierte Produkte - Bestimmung des biobasierten
carbone biosourcé des produits par la méthode du carbone Kohlenstoffanteils von Produkten mittels
radioactif Radiocarbonmethode
This Technical Specification (CEN/TS) was approved by CEN on 9 December 2013 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.





EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2014 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 16640:2014 E
worldwide for CEN national Members.

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SIST-TS CEN/TS 16640:2014
CEN/TS 16640:2014 (E)
Contents Page
Foreword .5
Introduction .6
1 Scope .7
2 Normative references .7
3 Terms and definitions .7
4 Symbols and abbreviations .9
5 Principle . 10
14
6 Determination of the C content . 11
6.1 General . 11
6.2 Principle . 11
6.3 Sampling . 11
6.4 Procedure for the conversion of the carbon present in the sample to a suitable sample for
14
C determination . 11
6.5 Measurements . 11
7 Calculation of the bio-based carbon content . 12
7.1 General . 12
7.2 Correction factors . 12
7.3 Calculation method. 13
7.3.1 Calculation of the bio-based carbon content by mass x . 13
B
TC
7.3.2 Calculation of the bio-based carbon content x as a fraction of TC . 14
B
TOC
7.3.3 Calculation of the bio-based carbon content x as a fraction of TOC . 14
B
7.3.4 Examples . 14
TC TOC
7.3.5 Examples of calculations of x and x . 15
B B
8 Test report . 16
Annex A (informative) Procedures for sampling of products . 17
A.1 General . 17
A.2 Solid samples . 17
A.2.1 General . 17
A.2.2 Plastics / polymers . 17
A.2.3 Fuels . 17
A.2.4 Ceramics / glass / concrete / cement / construction materials / waste . 17
A.2.5 Natural products . 18
A.3 Liquid samples . 18
A.3.1 General . 18
A.3.2 Solvents . 18
A.3.3 Fuels . 18
A.4 Gaseous samples . 19
2

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CEN/TS 16640:2014 (E)
A.5 Others . 19
Annex B (normative) Procedure for the conversion of the carbon present in the sample to a
14
C determination . 20
suitable sample for
B.1 General . 20
B.2 Sample preparation . 20
14
B.3 Preparation for C measurement . 21
B.3.1 General . 21
B.3.2 Reagents and materials . 22
B.4 Combustion of the sample in a calorimetric bomb . 22
B.4.1 Procedure . 22
B.4.2 Adsorption of the gas sample . 22
B.4.3 Combustion of the sample in a tube furnace or a combustion apparatus . 23
B.4.4 Dissolution and LSC direct measurement on the product . 23
Annex C (normative) Method A - Liquid scintillation-counter method (LSC) . 24
C.1 General . 24
C.2 Principle. 24
C.3 Reagents and materials . 24
C.4 Apparatus . 24
C.5 Procedure . 25
C.5.1 General . 25
C.5.2 Blank correction . 25
C.6 Calculation of the results. 26
Annex D (normative) Method B - Beta-ionization (BI) . 27
D.1 General . 27
D.2 Principle. 27
D.3 Reagents and materials . 27
D.4 Apparatus . 28
D.5 Procedure . 28
D.6 Calculation of the results. 29
Annex E (normative) Method C - Accelerator Mass Spectrometry (AMS) . 30
E.1 General . 30
E.2 Principle. 30
E.3 Reagents and materials . 30
E.4 Apparatus . 30
E.5 Procedure . 31
E.6 Calculation of the results. 31
14
Annex F (informative) Definitions and formulae of the C based method . 33
F.1 Introduction . 33
3

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CEN/TS 16640:2014 (E)
F.2 Symbols, abbreviations and definitions . 33
F.3 Principle of the method: How to determine the biogenic and fossil CO ratio of stack gas
2

samples . 34
14
F.4 Determination of standardized C values for the calculation of the biogenic and fossil
ratio of CO samples . 35
CO
2 2
F.4.1 General . 35
14
F.4.2 Standardization of C results for the three different measurement techniques . 35
F.5 Calculation of the biogenic carbon fraction . 39
F.5.1 General . 39
14
F.5.2 How to determine C and f . 39
otherC otherC
14
F.5.3 Definition of C . 39
bioC
Bibliography . 41



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SIST-TS CEN/TS 16640:2014
CEN/TS 16640:2014 (E)
Foreword
This document (CEN/TS 16640:2014) has been prepared by Technical Committee CEN/TC 411 “Bio-based
products”, the secretariat of which is held by NEN.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document has been prepared under Mandate M/492 "Mandate addressed to CEN, CENELEC and ETSI
for the development of horizontal European Standards and other standardization deliverables for bio-based
products".
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Croatia, Cyprus,
Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany,
Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.
5

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SIST-TS CEN/TS 16640:2014
CEN/TS 16640:2014 (E)
Introduction
Bio-based products from forestry and agriculture have a long history of application, such as paper, board and
various chemicals and materials. The last decades have seen the emergence of new bio-based products in
the market. Some of the reasons for the increased interest lie in the bio-based products’ benefits in relation to
the depletion of fossil resources and climate change. Bio-based products may also provide additional product
functionalities. This has triggered a wave of innovation with the development of knowledge and technologies
allowing new transformation processes and product development.
Acknowledging the need for common standards for bio-based products, the European Commission issued
1)
Mandate M/492 , resulting in a series of standards developed by CEN/TC 411, with a focus on bio-based
products other than food, feed and biomass for energy applications.
The standards of CEN/TC 411 "Bio-based products" provide a common basis on the following aspects:
— Common terminology
— Bio-based content determination
— Life Cycle Assessment (LCA)
— Sustainability aspects
— Declaration tools
Iit is important to understand what the term bio-based product covers and how it is being used. The term ‘bio-
based’ means 'derived from biomass'. Bio-based products (bottles, insulation materials, wood and wood
products, paper solvents, chemical intermediates, composite materials, etc.) are products which are wholly or
partly derived from biomass. It is essential to characterize the amount of biomass contained in the product by,
for instance, its bio-based content or bio-based carbon content.
The bio-based content of a product does not provide information on its environmental impact or sustainability,
which may be assessed through LCA and sustainability criteria. In addition, transparent and unambiguous
communication within bio-based value chains is facilitated by a harmonized framework for certification and
declaration.
This Technical Specification has been developed with the aim to specify the method for the determination of
14 14
bio-based carbon content in bio-based products using the C method. This method using the C method is
based on the analytical test methods used for the determination of the age of objects containing carbon.
This Technical Specification provides the reference test methods for laboratories, producers, suppliers and
purchasers of bio-based product materials and products. It may be also useful for authorities and inspection
organizations.
Part of the research leading to this document has been performed under the European Union Seventh
Framework Programme (see http://www.kbbpps.eu).This document is based on EN 15440 [1] prepared by
CEN/TC 343, "Solid recovered fuels", EN ISO 13833 [2], prepared by ISO/TC 146 "Air quality" and
CEN/TC 264 “Air quality", and CEN/TS 16137 [3], prepared by CEN/TC 249, "Plastics".
The analytical test methods specified in this Technical Specification are compatible with those described in
ASTM D 6866-12 [4].

1) A mandate is a standardization task embedded in European trade laws. Mandate M/492 is addressed to the European
Standardization bodies, CEN, CENELEC and ETSI, for the development of horizontal European Standards for bio-based
products.
6

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SIST-TS CEN/TS 16640:2014
CEN/TS 16640:2014 (E)
1 Scope
This Technical Specification specifies a method for the determination of the bio-based carbon content in
14
products, based on the C content measurement.
14
It also specifies three test methods to be used for the determination of the C content from which the bio-
based carbon content is calculated:
— Method A: Liquid scintillation-counter method (LSC);
— Method B: Beta-ionization (BI);
— Method C: Accelerator mass spectrometry (AMS).
The bio-based carbon content is expressed by a fraction of sample mass, as a fraction of the total carbon
content or as a fraction of the total organic carbon content.
This calculation method is applicable to any product containing organic carbon, including biocomposites.
NOTE This Technical Specification does not provide the methodology for the calculation of the biomass content of a
sample.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
EN 15400, Solid recovered fuels — Determination of calorific value
EN ISO 1716, Reaction to fire tests for products — Determination of the gross heat of combustion (calorific
value) (ISO 1716)
ISO 1928, Solid mineral fuels — Determination of gross calorific value by the bomb calorimetric method, and
calculation of net calorific value
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
bio-based carbon content
fraction of carbon derived from biomass in a product
Note 1 to entry:  There are several approaches to express the bio-based carbon content. These include as a
percentage of: the mass; the total carbon content, or the total organic carbon content, of the sample. These are detailed in
the relevant standards of CEN/TC 411.
[SOURCE: prEN 16575:2013 [5]]
3.2
biomass content
see bio-based content
[SOURCE: prEN 16575:2013 [5]]
7

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CEN/TS 16640:2014 (E)
3.3
bio-based content
fraction of a product that is derived from biomass
Note 1 to entry: Normally expressed as a percentage of the total mass of the product.
Note 2 to entry: For the methodology to determine the bio-based content, see TC 411 WI 00411002 bio-based
content.
[SOURCE: prEN 16575:2013 [5]]
3.4
organic material
material containing carbon-based compound in which the element carbon is attached to other carbon atoms,
hydrogen, oxygen, or other elements in a chain, ring, or three-dimensional structure
3.5
organic carbon
carbon from organic material
3.6
isotope abundance
fraction of atoms of a particular isotope of an element
3.7
percentage modern carbon
pMC
14
normalized and standardized value for the amount of the C isotope in a sample, calculated relative to the
14
2)
standardized and normalized C isotope amount of oxalic acid standard reference material, SRM 4990c
Note 1 to entry: In 2009, the value of 100 % bio-based carbon was set at 105 pMC.
3.8
laboratory sample
sub-quantity of a sample suitable for laboratory tests
3.9
sample
quantity of material, representative of a larger quantity for which the property is to be determined
3.10
sample preparation
all the actions taken to obtain representative analysis samples or test portions from the original sample
3.11
beta- particle
electron emitted during radioactive decay
3.12
total carbon
TC
quantity of carbon present in a product in the form of organic, inorganic and elemental carbon
[SOURCE: prEN 16575:2013 [5]]

2) SRM 4990c is the trade name of a product supplied by the US National Institute of Standards and Technology. This
information is given for the convenience of users of this document and does not constitute an endorsement by
CEN of this product. Equivalent products may be used if they can be shown to lead to the same results.
8

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CEN/TS 16640:2014 (E)
3.13
total organic carbon
TOC
quantity of organic carbon present in a product
Note 1 to entry: Total organic carbon is often determined as the carbon that is converted into carbon dioxide by
combustion and which is not liberated as carbon dioxide by acid treatment.
[SOURCE: prEN 16575:2013 [5]]
4 Symbols and abbreviations
14
C carbon isotope with an atomic mass of 14
AMS accelerator mass spectrometry
BI beta-ionization
Bq Bequerel (disintegrations per second)
C symbol for element carbon
cpm counts per minute
dpm disintegrations per minute
GM Geiger-Müller
LLD lower limit of detection
LSC Liquid Scintillation Counter or Liquid Scintillation Counting
m mass of a sample expressed in grams
MOP 3-methoxy 1-propyl amine
PE polyethylene
PLA poly(lactic acid)
pMC percentage of modern carbon
pMC(s) measured value, expressed in pMC, according to AMS method, of the sample
REF reference value, expressed in pMC, of 100 % bio-based carbon depending on the origin of
organic carbon
TC total carbon
TOC total organic carbon
x bio-based carbon content by mass, expressed as a percentage of the mass of the sample
B
TC
x total carbon content, expressed as a percentage of the mass of the sample
9

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SIST-TS CEN/TS 16640:2014
CEN/TS 16640:2014 (E)
TC
bio-based carbon content by total carbon content, expressed as a percentage of the total carbon
x
B

content
TOC
x total organic carbon content, expressed as a percentage of the mass of the sample
TOC
bio-based carbon content by total organic carbon content, expressed as a percentage of the
x
B

total organic carbon content
5 Principle
14
The C present in products is originating from recent atmospheric CO . Due to its radioactive decay, it is
2
14
almost absent from fossil products older than 20 000 years to 30 000 years. The C content may thus be
considered as a tracer of products recently synthesized from atmospheric CO and particularly of recently
2
produced bio-products.
14
The determination of the biomass content is based on the measurement of C in bio-based products which
allows the calculation of the bio-based carbon fraction.
14
A large experience in C determination and reference samples is available from dating of archaeological
objects, on which the three methods described in this technical specification are based:
— Method A: Proportional scintillation-counter method (LSC),
— Method B: Beta-ionization (BI), or
— Method C: Accelerator mass spectrometry (AMS).
NOTE The advantages and disadvantages of these test methods are given in Table 1.
Table 1 — Advantages and disadvantages of the methods
Method Technical Additional Duration needed Relative Instrumental
level requests for measurement standard costs
deviation
Method A Simple Normal laboratory 4 h to 12 h 2 % to 10 % Low
(LSC)
Method B (BI) Complex - Low background 8 h to 24 h 0,2 % to 5 % Low
laboratory
- Gas purification
device
Method C Very - Large installation 10 min to 30 min 0,2 % to 2 % High
(AMS) complex
- Graphite
Conversion device
14
For the C LSC measurement a Low Level Counter should be used. The statistical scattering of the
radioactive decay sets a limit, both for method A and B. Thereby both methods need a purified carbon dioxide,
otherwise oxides of nitrogen from the combustion in the calorific bomb will result in counting losses by
quenching and adulteration of the cocktail in case of LSC measurement.
10

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CEN/TS 16640:2014 (E)
14
6 Determination of the C content
6.1 General
14
A general sample preparation and three test methods for the determination of the C content are described in
this Technical Specification. With this modular approach, it will be possible for normally equipped laboratories
14 14
to prepare samples for the C content, and determine the C content with own equipment or to outsource the
14
determination of the C content to laboratories that are specialized in this technique.
14
For the collection from the sample of the C content, generally accepted methods for the conversion of the
carbon present in the sample to CO are described.
2
14
For the measurement of the C content, methods are selected that are already generally accepted as
methods for the determination of the age of objects.
6.2 Principle
14
The amount of bio-based carbon in the bio-based product is proportional to this C content.
Complete combustion (see Annex B) is carried out in a way to comply with the requirements of the
14
subsequent measurement of the C content and shall provide the quantitative recovery of all carbon prese
...

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