CEN/TS 16640:2014

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

This Technical Specification 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 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.

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: 29-Jun-2014
• Withdrawal Date: 21-Feb-2017
• ICS: 13.020.55 - Biobased products
• ICS: 13.020.60 - Product life-cycles
• ICS: 71.040.40 - Chemical analysis
• ICS: 83.040.01 - Raw materials for rubber and plastics in general
• Technical Committee: CEN/TC 411 - Bio-based products
• Drafting Committee: CEN/TC 411/WG 3 - Bio-based content
• Current Stage: 9960 - Withdrawal effective - Withdrawal
• Completion Date: 22-Feb-2017
• Mandate: M/492 - Mandate addressed to CEN, CENELEC and ETSI for the development of European standards and other standardisation deliverables for bio-based products
• Ref Project: SIST-TS CEN/TS 16640:2014 - Bio-based products - Determination of the bio based carbon content of products using the radiocarbon method

Relations

• Replaced By: EN 16640:2017 - Bio-based products - Bio-based carbon content - Determination of the bio-based carbon content using the radiocarbon method
• Effective Date: 01-Mar-2017

Standards Content (Sample)

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
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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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

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

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

7.3.2 Calculation of the bio-based carbon content x as a fraction of TC ........................................... 14

TOC

7.3.3 Calculation of the bio-based carbon content x as a fraction of TOC ...................................... 14

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

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A.5 Others ................................................................................................................................................... 19

Annex B (normative) Procedure for the conversion of the carbon present in the sample to a

C determination ............................................................................................... 20

suitable sample for

B.1 General ................................................................................................................................................. 20

B.2 Sample preparation ............................................................................................................................. 20

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

Annex F (informative) Definitions and formulae of the C based method ................................................. 33

F.1 Introduction .......................................................................................................................................... 33

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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

samples ................................................................................................................................................ 34

F.4 Determination of standardized C values for the calculation of the biogenic and fossil

ratio of CO samples ................................................................................................................... 35

2 2

F.4.1 General ................................................................................................................................................. 35

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

F.5.2 How to determine C and f .............................................................................................. 39

otherC otherC

F.5.3 Definition of C ............................................................................................................................. 39

bioC

Bibliography ..................................................................................................................................................... 41

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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.

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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

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.
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1 Scope

This Technical Specification specifies a method for the determination of the bio-based carbon content in

products, based on the C content measurement.

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]]
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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

normalized and standardized value for the amount of the C isotope in a sample, calculated relative to the

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

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.

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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
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

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

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

total organic carbon content
5 Principle

The C present in products is originating from recent atmospheric CO . Due to its radioactive decay, it is

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

produced bio-products.

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.

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

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.
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6 Determination of the C content
6.1 General

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

determination of the C content to laboratories that are specialized in this technique.

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.

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

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

subsequent measurement of the C content and shall provide the quantitative recovery of all carbon prese

...