Wood and wood based products - Dosage of the total organic carbon (TOC) in wood and wood based products

This document describes a method for determining total organic carbon by calculating the difference between the results of measurements of total carbon (TC) and total inorganic carbon (TIC). The identification of the bio-based content given by the stable isotopes such as 13C is described also.
This method is applicable to all wood species, wood-based materials (panels, plywood, wood-polymer, etc.) and woods containing chemicals in general.

Holz und Holzprodukte - Bestimmung des gesamten organischen Kohlenstoffs (TOC) in Holz und Holzprodukten

Dieses Dokument beschreibt ein Verfahren zur Bestimmung des gesamten organischen Kohlenstoffs durch Berechnung der Differenz zwischen den Messergebnissen des gesamten Kohlenstoffs (TC) und des gesamten anorganischen Kohlenstoffs (TIC). Die Identifizierung des durch die stabilen Isotope, wie 13C, festgestellten biobasierten Gehalts wird ebenfalls beschrieben.
Dieses Verfahren ist für alle Holzarten, Holzprodukte (Platten, Sperrholz, Holzpolymer usw.) und die in Hölzern im Allgemeinen enthaltenen Chemikalien anwendbar.

Produits de préservation du bois et matériaux à base de bois - Dosage du carbone organique total (COT) dans les bois et matériaux à base de bois

Le présent document décrit une méthode de détermination du carbone organique total par calcul de la différence entre les résultats des mesures de carbone total (CT)  et du carbone inorganique total (CI). Il décrit également l'identification du contenu biosourcé indiqué par les isotopes stables tels que 13C.
Cette méthode est applicable sur toutes les essences de bois, les matériaux à base de bois (panneaux, contre-plaqués, bois-polymères, etc.) et les bois contenant des produits chimiques en général.

Les in lesni proizvodi - Delež celotnega organskega ogljika (TOC) v lesu in lesnih proizvodih

Ta dokument opisuje metodo za ugotavljanje skupnega organskega ogljika z izračunom razlike med rezultati merjenja skupnega ogljika (TC) in skupnega anorganskega ogljika (TIC). Opisuje tudi identifikacijo biološke vsebine, ki jo podajajo stabilni izotopi, kot je 13C.
Metoda splošno velja za vse lesne vrste, materiale na osnovi lesa (plošče, vezan les, lesni polimer itd.) in les, ki vsebuje kemikalije.

General Information

Status
Published
Public Enquiry End Date
29-Sep-2015
Publication Date
21-Dec-2015
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
11-Dec-2015
Due Date
15-Feb-2016
Completion Date
22-Dec-2015

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SLOVENSKI STANDARD
SIST EN 16718:2016
01-februar-2016

Les in lesni proizvodi - Delež celotnega organskega ogljika (TOC) v lesu in lesnih

proizvodih

Wood and wood based products - Dosage of the total organic carbon (TOC) in wood and

wood based products

Holz und Holzprodukte - Bestimmung des gesamten organischen Kohlenstoffs (TOC) in

Holz und Holzprodukten
Produits de préservation du bois et matériaux à base de bois - Dosage du carbone
organique total (COT) dans les bois et matériaux à base de bois
Ta slovenski standard je istoveten z: EN 16718:2015
ICS:
79.040 Les, hlodovina in žagan les Wood, sawlogs and sawn
timber
79.060.01 /HVQHSORãþHQDVSORãQR Wood-based panels in
general
SIST EN 16718:2016 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 16718:2016
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SIST EN 16718:2016
EN 16718
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2015
EUROPÄISCHE NORM
ICS 79.060.01
English Version
Wood and wood based products - Dosage of the total
organic carbon (TOC) in wood and wood based products

Produits de préservation du bois et matériaux à base Holz und Holzprodukte - Bestimmung des gesamten

de bois - Dosage du carbone organique total (COT) organischen Kohlenstoffs (TOC) in Holz und

dans les bois et matériaux à base de bois Holzprodukten
This European Standard was approved by CEN on 12 September 2015.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

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

© 2015 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 16718:2015 E

worldwide for CEN national Members.
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SIST EN 16718:2016
EN 16718:2015 (E)
Contents Page

European foreword ....................................................................................................................................................... 4

Introduction .................................................................................................................................................................... 5

1 Scope .................................................................................................................................................................... 7

2 Normative references .................................................................................................................................... 7

3 Terms and definitions ................................................................................................................................... 7

4 Principle ............................................................................................................................................................. 7

5 Reagents and products .................................................................................................................................. 8

6 Apparatus ........................................................................................................................................................... 8

7 Procedure........................................................................................................................................................... 8

7.1 Preparation of the sample ........................................................................................................................... 8

7.2 Water content ................................................................................................................................................... 8

7.3 Dosage ................................................................................................................................................................. 9

7.3.1 General ................................................................................................................................................................ 9

7.3.2 TC dosage ........................................................................................................................................................... 9

7.3.3 TIC dosage .......................................................................................................................................................... 9

7.4 Calibration ......................................................................................................................................................... 9

7.5 Control measurements ............................................................................................................................... 10

7.6 Evaluation ....................................................................................................................................................... 10

7.7 C measurement by IRMS (Isotope Ratio Mass Spectrometer) .................................................. 11

7.7.1 Material and methods ................................................................................................................................. 11

7.7.2 C isotope ....................................................................................................................................................... 12

7.7.3 O isotope ...................................................................................................................................................... 12

7.7.4 H isotope (Deuterium) .............................................................................................................................. 12

7.7.5 N Isotopes .................................................................................................................................................... 12

13 18 2

7.7.6 Multi-isotopic determinations: C, O and H in wood and tree ............................................... 12

8 Performance characteristics .................................................................................................................... 13

9 Test report ...................................................................................................................................................... 13

Annex A (informative) Results of the validation method ........................................................................... 14

A.1 General ............................................................................................................................................................. 14

A.2 Response function ........................................................................................................................................ 14

A.2.1 General ............................................................................................................................................................. 14

A.2.2 Total carbon ................................................................................................................................................... 15

A.2.3 Inorganic carbon .......................................................................................................................................... 16

A.3 Trueness .......................................................................................................................................................... 17

A.3.1 General ............................................................................................................................................................. 17

A.3.2 Total carbon ................................................................................................................................................... 18

A.3.3 Inorganic carbon .......................................................................................................................................... 18

A.4 Precision .......................................................................................................................................................... 18

A.4.1 General ............................................................................................................................................................. 18

A.4.2 Total carbon ................................................................................................................................................... 18

A.4.3 Inorganic carbon .......................................................................................................................................... 20

A.5 Measurement uncertainty ........................................................................................................................ 21

A.5.1 General ............................................................................................................................................................. 21

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EN 16718:2015 (E)

A.5.2 Total carbon.................................................................................................................................................... 21

A.5.3 Inorganic carbon ........................................................................................................................................... 22

A.6 Accuracy ........................................................................................................................................................... 22

A.6.1 General ............................................................................................................................................................. 22

A.6.2 Total carbon.................................................................................................................................................... 22

A.6.3 Inorganic carbon ........................................................................................................................................... 24

A.7 Linearity of results ....................................................................................................................................... 25

A.7.1 Total carbon.................................................................................................................................................... 25

A.7.2 Inorganic carbon ........................................................................................................................................... 26

A.8 Quantification limit and dosage interval ............................................................................................. 27

A.8.1 Total carbon.................................................................................................................................................... 27

A.8.2 Inorganic carbon ........................................................................................................................................... 27

A.9 Conclusion ....................................................................................................................................................... 27

Annex B (informative) Measurements on wood species and wood-based materials ....................... 28

Bibliography ................................................................................................................................................................. 29

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SIST EN 16718:2016
EN 16718:2015 (E)
European foreword

This document (EN 16718:2015) has been prepared by Technical Committee CEN/TC 38 “Durability of

wood and wood-based products”, the secretariat of which is held by AFNOR.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by May 2016, and conflicting national standards shall be

withdrawn at the latest by May 2016.

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.

According to the CEN/CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: 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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SIST EN 16718:2016
EN 16718:2015 (E)
Introduction

Bio-based products from forestry and agriculture have a long history of application. The last decades

have seen the emergence of new bio-based products in the market. 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.

For business to business transactions, claims which are relevant to describe characteristics of bio-based

products in a business to business environment will be given in the near future. Data are by

consequence required to generate and transfer information in the industrial chain and/or as an input

for product specific standards and certification schemes.

The work to be done by the CEN/TC 411/WG 3 concerns the determination of the bio-based carbon in

order to determine the level of bio-based content of a product or materials. A document

(CEN/TR 16721) has been prepared by Technical Committee CEN/TC 411 “Bio-based products”, and

describes a list of methods and an “overview of methods to determine the bio-based content and related

methods” for Bio-based products.

As part of the task force of CEN/TC 175, devoted to carbon foot printing and LCA, a European Standard

was published on the simplified calculation of the amount of biomass carbon stored in wood (using

50 % of the anhydrous wood mass): EN 16449.

This standard EN 16718 describes the methods based on analytical measurements. These methods can

be considered as complementary to the radiocarbon based method and methods based on evaluation by

calculation (mass balance approaches). One of these analytical methods is a method based on

measurement of stable isotopic ratio present in biomass in order to determine the biomass content of

the product.

The development of this method described in this report is ongoing with close collaboration between

FCBA and the “Institute des Sciences Analytiques” CNRS in order to determine the bio-based content of

wood raw materials, glues and panels made with these raw materials for end use manufactured

products with this new method. The objective is to propose correlated analysis (with the TOC method

proposed by FCBA) to determine the carbon content to purpose a quick and low cost method easy to

handle.
References:
— http://www.biobasedeconomy.eu/standardisation/cen-tc411/
— http://www2.afnor.org/espace_normalisation/structure.aspx?commid=86489

The tests that have resulted in the specification of this document were performed in the context of work

conducted by the FCBA [timber certification body] Technological Institute aimed at determining a

method for supplying data on organic carbon contents that could be used to calculate carbon balances.

The storage of biomass carbon in wood-based products is the preservation of the carbon absorbed by

the tree from atmospheric CO through photosynthesis.

The carbon thus captured in the material is of benefit to the climate throughout the lifespan of the

product, which can be several dozen years for a construction product, for example. The French Standard

NF P01-010 (2004), which lays out the format of environmental and health statements (FDES) for

construction products, provides the option of indicating the following supplementary information, in

addition to the “Climate change” indicator, which is calculated from the flows of greenhouse gases

associated with the product life cycle: “for some construction products (e.g. plant-based products), CO2

storage during the “service life” stage can be given if measurements are taken based on standardized

test methods.”
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EN 16718:2015 (E)

Furthermore, the Guide to Best Practices on environmental labelling of mass-market consumer

products (BP X30-323) includes in Annex G: “Carbon accounting integrating time lag” which also

requires knowledge of the biomass carbon contents of the products.

The purpose of this document is therefore to propose a laboratory measurement method of the amount

of biomass carbon that will provide values of carbon or CO equivalent stored in wood-based products,

with the aim to integrate this information in the environmental statements of these products according

to the texts referenced above.

While measurement is not systematically necessary for solid wood products, for example, given the

common knowledge on the densities of the various wood species and on the proportion of carbon

contained in wood, this experimental measurement may prove to be necessary for products made of

wood-based composite materials.

The organic carbon contained in wood and wood-based materials is found in several different forms.

Cumulative measurements, such as total organic carbon (TOC), need to be used. Isotopic ratio enables

the differentiation between synthetic and natural products. IRMS (Isotope Ratio Mass Spectrometer) is

a complementary method to the TOC method by an identification of the isotope C: both techniques are

necessary to give reliable data on a bio-based content on a wood based material such as panel, board,

and woods containing chemicals in general. A study is currently in progress in France on wood based

materials: the results will enable to improve this present document and to give data with multi-isotopic

13 15 2 18
determinations ( C, N, H, O).
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SIST EN 16718:2016
EN 16718:2015 (E)
1 Scope

This European Standard describes a method for determining total organic carbon by calculating the

difference between the results of measurements of total carbon (TC) and total inorganic carbon (TIC).

The identification of the bio-based content given by the stable isotopes such as C is described also.

This method is applicable to all wood species, wood-based materials (panels, plywood, wood-polymer,

etc.) and woods containing chemicals in general.
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 13183-1, Moisture content of a piece of sawn timber — Part 1: Determination by oven dry method

3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
total carbon
amount of carbon found in waste, in organic, inorganic and elemental-state forms
3.2
total inorganic carbon
TIC
amount of carbon released as carbon dioxide through acidification
3.3
total organic carbon
TOC

carbon that is transformed into carbon dioxide through combustion and not released through

acidification as carbon dioxide

Note 1 to entry: The definitions given above are only applicable in this document and only partly overlap the

scientific definitions of TC, TOC and TIC.
4 Principle

In this procedure, TOC is obtained by subtraction between the measurement results of TC and TIC.

The total carbon (TC) present in the undried sample is transformed into carbon dioxide through

combustion in a flow of gas that contains oxygen and is free of carbon dioxide. To ensure combustion is

total, catalysers and/or modifiers can be used. The amount of carbon dioxide released is measured

using infrared spectrometry, gravimetry, coulometry, conductometry, thermal conductivity detection or

flame ionization detection after reduction to methane, or any other appropriate technique.

The TIC is determined separately using another sub-sample, through acidification and purging of the

released carbon dioxide, which is then measured using one of the techniques mentioned above.

The C identification by IRMS is described in 7.7. This protocol is able also to work on other isotopes:

15 2 18
N, H and O, which could be useful for complex materials containing wood.
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SIST EN 16718:2016
EN 16718:2015 (E)
5 Reagents and products

All the reagents used shall be of analytical grade at least and suitable for their specific uses. Hygroscopic

products shall be kept in a dessicator.
5.1 Glucose, C H O .
6 12 6
5.2 Anhydrous sodium carbonate, Na CO .
2 3

5.3 Non-oxidizing mineral acid used to release the carbon dioxide, e.g. phosphoric acid H PO ,

3 4
(m = 85 %).

5.4 Synthetic air, nitrogen, oxygen, argon, free of carbon dioxide and organic impurities,

according to the instructions supplied by the machine manufacturer.
6 Apparatus
6.1 Homogenization device, such as mixers, stirrers.
6.2 Analytical balance accurate to at least 0,5 % of test portion weight.
6.3 Apparatus for dosing carbon in solid matter, along with its accessories.
6.4 Purging device for dosing TIC.
6.5 Mixer mill.
7 Procedure
7.1 Preparation of the sample

Before the sample preparation, the sampling program shall be properly designed in accordance with the

context of the testing and objectives.
The samples to be analysed should be as homogeneous as possible and undried.

The samples of wood or wood-based materials can be directly ground (avoiding any heating) and

reduced to powder, preferably with a particle size below 500 μm. The samples are ground in their

entire thickness.

The samples that contain negligible concentrations (taking into account the accuracy of the method

used) of volatile compounds other than water can be dried at 105 °C before they are homogenized.

7.2 Water content

The determination of moisture content shall be carried out using a different test portion. It can be

calculated from the dry matter mass, determined according to EN 13183-1.

NOTE Any other determination method (e.g. with a desiccator’s balance) can be used if it has been previously

validated.
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EN 16718:2015 (E)
7.3 Dosage
7.3.1 General

This document does not give any recommendations for the apparatus and its mode of operation. The

operating conditions should be selected and verified according to the instructions supplied by the

manufacturer.

It is advisable to select a test portion with the greatest mass possible, making sure that the amount of

carbon dioxide released is within the apparatus measurement range and the calibration range.

7.3.2 TC dosage

The sample, prepared according to 7.1, is weighed in an appropriate container, i.e. inert and not liable to

interact during the carbon content analysis reaction or to contain carbon in any form whatsoever

(scoop or crucible made of e.g. ceramic, silica glass, platinum or tin). The container can be previously

conditioned by heating (in a muffle furnace or in the analyser itself) to minimize blank carbon values.

The sample is burned or broken down in a carrier gas current that contains oxygen.

The combustion temperature shall be sufficiently high to transform all the carbon into carbon dioxide.

For samples containing carbonates that are difficult to break down, such as barium carbonate, carbon

dioxide release can be improved by increasing the temperature or using modifiers (e.g. tin, copper).

The temperature range of commercially available devices is between 900 °C and 1 500 °C.

During combustion of the reactive samples, any detonation or production of smoke can be avoided by

covering the sample with an inert material (e.g. siliceous sand).

The carbon dioxide released while gas is being discharged is measured using the detection method

described in chapter 4, and expressed as carbon.
7.3.3 TIC dosage
The sample prepared according to 7.1 is weighed in the purging device.

The system is closed so as to be impermeable to gases and purged using the carrier gas until the carbon

dioxide from the ambient air is eliminated. Then, acid is added and the carbon dioxide is carried out

through purging or stirring and/or heating. The carbon dioxide released is transferred to the detector

by means of the carrier gas.

The carbon dioxide released while gas is being discharged is measured using the detection method

described in Clause 4, and expressed as carbon.
7.4 Calibration

If detection is carried out using a relative method, e.g. infrared detection, calibration is necessary.

Glucose is an example of a standard substance that is appropriate for TC dosage.
Sodium carbonate or calcium carbonate can be used for TIC calibration.

Other standard substances can be used, provided their suitability has been verified.

During calibration, the procedure below should be followed:
— set the preliminary measurement range;

— analyse a series of four calibration samples minimum at least twice, at three different times. The

concentration of these master samples shall be regularly distributed over the entire measurement

range;
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SIST EN 16718:2016
EN 16718:2015 (E)
— calculate the mean values for each concentration;
— perform a linear regression analysis using the mean values.

This function should be linear. If this is not the case, the measurement range needs to be reduced to the

linear range.

This calibration should not be implemented for initial validation purposes or when major modifications

of the apparatus are carried out.
7.5 Control measurements

Control measurements shall be taken to make sure the apparatus is functioning properly. They should

be taken every working day. It is deemed sufficient to perform the dosage three times from a point

located in the middle of the respective measurement ranges. For TC and TIC, the mean recovery rate

shall be between 90 % and 110 % with a variation coefficient ≤ 5 %.
7.6 Evaluation

The TC and TIC masses contained in the samples prepared according to 7.1 are calculated using:

— The calibration function and the sample mass where relative detection methods are used;

— Specific constants and the sample mass where absolute detection methods are used.

TC and TIC contents are the means of at least two measurements each. The respective differences

between the two values should be less than or equal to 10 % of the mean value. If this is not the case, at

least one other additional dosage needs to be carried out; in such a case, the variation coefficient should

be less than or equal to 10 %. If this is not the case, the coefficient shall be recorded along with the

result obtained.

The TOC content is calculated using the difference between the mean TC and TIC values with the

following formula:
ω ωω− (1)
TOC TC TIC
where

ω is the TOC content in carbon dioxide form in the original sample, in grams per kilogram (g/kg);

TOC

ω is the mean value of the TC content in carbon dioxide form in the sample, in grams per kilogram

(g/kg);

ω is the mean value of the TIC content in carbon dioxide form in the sample, in grams per kilogram

TIC
(g/kg).

The TOC content yielded by Formula (1) is correlated to the dry matter using Formula (2). To do so, the

water content, determined separately, is used:
100
ω =ω (2)
TOCdm TOC
100−w
where

ω is the TOC content in carbon dioxide form, correlated to the dry matter base, in grams per kilogram

TOCdm
(g/kg);

is the TOC content in carbon dioxide form in the original sample, in grams per kilogram (g/kg);

TOC

w is the water content of the original sample, expressed as a mass fraction in percentage (%).

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EN 16718:2015 (E)

The TOC content is generally determined using the undried sample, but it is always recorded as carbon

correlated to dry matter. With Formula (2), the results are obtained in g/kg. They can be converted to

other units by using the app
...

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