SIST EN 15440:2011

Solid recovered fuels - Method of the determination of biomass content

This European Standard specifies three normative methods for the determination of the biomass fraction in solid recovered fuel, and when to use each method. The methods are the selective dissolution in a hydrogen peroxide/sulphuric acid mixture, the manual sorting method and the method based on the 14C content.

Feste Sekundärbrennstoffe - Verfahren zur Bestimmung des Gehaltes an Biomasse

Diese Europäische Norm legt drei normative Verfahren zur Bestimmung des Biomasse-Anteils in festen Sekundärbrennstoffen fest und wann welches Verfahren anzuwenden ist. Die drei Verfahren sind die selektive Auflösung in einem Wasserstoffperoxid-/Schwefelsäure-Gemisch, das Verfahren der manuellen Sortierung und das Verfahren auf der Grundlage des 14C-Gehaltes.

Combustibles solides de récupération - Méthode de détermination de la teneur en biomasse

La présente Norme européenne spécifie trois méthodes normatives pour déterminer la fraction de biomasse dans un combustible solide de récupération et le moment où utiliser chaque méthode. Les méthodes sont la dissolution sélective dans un mélange peroxyde d'hydrogène/acide sulfurique, la méthode du tri manuel et la méthode basée sur la teneur en 14C.

Trdna alternativna goriva - Metoda za določevanje biomase

Ta evropski standard določa tri normativne metode za določevanje frakcije biomase v trdnih alternativnih gorivih in kdaj se vsaka od metod uporablja. Metode so selektivno raztapljanje v mešanici vodikovega peroksida/žveplove kisline, metoda z ročnim razvrščanjem in metoda, ki temelji na vsebnosti 14C.

General Information

• Status: Withdrawn
• Public Enquiry End Date: 30-Aug-2009
• Publication Date: 07-Apr-2011
• Withdrawal Date: 04-Feb-2021
• ICS: 27.190 - Biological sources and alternative sources of energy
• ICS: 75.160.10 - Solid fuels
• Technical Committee: AGO - Refuse derived fuel
• Current Stage: 9900 - Withdrawal (Adopted Project)
• Start Date: 03-Feb-2021
• Due Date: 26-Feb-2021
• Completion Date: 05-Feb-2021
• Mandate: M/325 - Mandate to CEN on Solid Recovered Fuels (SRF)
• Ref Project: EN 15440:2011 - Solid recovered fuels - Methods for the determination of biomass content

Relations

• Replaces: SIST-TS CEN/TS 15440:2007 - Solid recovered fuels - Method for the determination of biomass content
• Effective Date: 01-May-2011
• Replaces: SIST-TS CEN/TS 15747:2009 - Solid recovered fuels - 14C-based methods for the determination of the biomass content
• Effective Date: 01-May-2011
• Replaced By: SIST EN ISO 21644:2021 - Solid recovered fuels - Methods for the determination of biomass content (ISO 21644:2021, Corrected version 2021-03)
• Effective Date: 01-Mar-2021
• Corrected By: SIST EN 15440:2011/AC:2011 - Solid recovered fuels - Methods for the determination of biomass content
• Effective Date: 01-Dec-2011

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Feste Sekundärbrennstoffe - Verfahren zur Bestimmung des Gehaltes an BiomasseCombustibles solides de récupération - Méthode de détermination de la teneur en biomasseSolid recovered fuels - Method of the determination of biomass content75.160.10Trda gorivaSolid fuelsICS:Ta slovenski standard je istoveten z:EN 15440:2011SIST EN 15440:2011en,de01-maj-2011SIST EN 15440:2011SLOVENSKI
STANDARDSIST-TS CEN/TS 15747:2009SIST-TS CEN/TS 15440:20071DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15440
March 2011 ICS 75.160.10 Supersedes CEN/TS 15440:2006, CEN/TS 15747:2008English Version
Solid recovered fuels -Methods for the determination of biomasscontent
Combustibles solides de récupération - Méthode de détermination de la teneur en biomasse
Feste Sekundärbrennstoffe - Verfahren zur Bestimmung des Gehaltes an Biomasse This European Standard was approved by CEN on 22 January 2011.
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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15440:2011: ESIST EN 15440:2011

Determination of biomass content using the selective dissolution method . 14Annex B (normative)
Determination of biomass content using the manual sorting method . 23Annex C (normative)
Determination of the biomass content based on the 14C method . 29Annex D (informative)
Limitations of the determination methods . 48Annex E (informative)
Materials considered as CO2-neutral . 52Annex F (informative)
Performance data . 53Bibliography . 56 SIST EN 15440:2011

(ISO/IEC 17025:2005) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 15357:2011 and the following apply. 3.1 ash content inorganic mass remaining after complete combustion of a solid recovered fuel under specified conditions expressed as a percentage of the mass of the dry matter in the solid recovered fuel 3.2 biodegradable material capable of undergoing biological anaerobic or aerobic decomposition under conditions naturally occurring in the biosphere NOTE (Council Directive 1999/31/EC on the landfill of biodegradable waste; any waste that is capable of undergoing anaerobic or aerobic decomposition, such as food and garden waste, and paper and paperboard.)
1) To be published. SIST EN 15440:2011

2) No definition. SIST EN 15440:2011

The old term for total moisture is moisture content. 3.11 net calorific value calculated value of the specific energy of combustion for unit mass of a solid recovered fuel burned in oxygen in calorimetric bomb under such conditions that all the water remains as water vapor at 0,1 MPa NOTE
The old term for net calorific value is lower heating value. 3.12 nominal minimum size aperture size of the sieve used for determining the particle size distribution of solid recovered fuels through which no more than 5 % by mass of the material passes 3.13 nominal top size aperture size of the sieve used for determining the particle size distribution of solid recovered fuels through which at least 95 % by mass of the material passes
3.14 percentage modern Carbon (pmC) percent modern carbon relative to the NIST Oxalic acid standard reference material SRM4990B NOTE 1 The internationally accepted radiocarbon dating reference value is 95 percent of the activity, in AD 1950, of this NBS oxalic acid SRM4990B. NOTE 2 In 2008 the value of 100 % biogenic carbon is set at 107 pmC. 3.15 sample quantity of material, representative of a larger quantity for which the property is to be determined 3.16 sample preparation all actions taken to obtain representative analyses samples or test portions from the original sample 3.17 sub-sample sample obtained by procedures in which the items of interest are randomly distributed in parts of equal or unequal size NOTE 1 A sub-sample can be: d) a portion of the sample obtained by selection or division; e) the final sample of multistage sample-preparation. NOTE 2
The definition for sub-sample is adopted from CEN/TC 292. SIST EN 15440:2011

Directive 2001/77/EC of the European parliament and council of 27 September 2001 RSD Relative standard deviation SDM Selective dissolution method SRF Solid recovered fuel TC Total carbon content X Fraction expressed as a percentage by weight. Expressions to different bases employed in this document are given with the suffixes:
(ad) for air-dried:
(ar)
for as received:
(d) for dry:
(daf) for dry and ash free, where appropriate. Example; calNB(d)x means the fraction of energy content in the non-biomass fraction, on dry basis 5 Principle The determination of the biomass content is based on selective dissolution, manual sorting or 14C measurement of biomass in solid recovered fuel. The choice for the method to be used is described in the next clause. The biomass content gives an estimation of the content of the biodegradable/biogenic fraction in solid recovered fuel. 6 Determination of biomass content 6.1 Sampling Sampling, transport, storage of the solid recovered fuel and sample preparation in the field shall be conducted according to EN 15442 and EN 15443. Preparation of the test sample shall be conducted according to
EN 15413. 6.2 Applicable methods For the determination of biomass content three methods are available: 1) the determination of the biomass content based on the selective dissolution method (SDM) (see Annex A). The determination of the biomass content based on the selective dissolution method is based on the property of biomass that it can be dissolved in a sulphuric acid / hydrogen peroxide mixture; 2) the determination of the biomass content based on the manual sorting method (MS). This method is suitable for samples with a particle size > 10 mm (see Annex B); SIST EN 15440:2011

14C / SDM
NOTE 1 The determination of the biomass fraction with 14C expressed by energy content has not been validated. NOTE 2 The MS combined with the CV determination or the TC determination of the biomass and the non-biomass fraction could be used for internal analyses. In Table 1 [RES-E] refers to Directive 2001/77/EC of the European parliament and council of 27 September 2001 on the promotion of electricity produced from renewable energy sources in the internal electricity market and [CO2 trading] refers to greenhouse gas reduction related issues. Figure 1 gives a decision tree for finding the right method for the determination. SIST EN 15440:2011

where MS = Manual sorting SDM = Selective dissolution method 14C = Radiocarbon method D05 = nominal minimum size Figure 1 — Decision tree for the selection of determination method NOTE 3 The MS combined with the CV determination or the TC determination of the biomass and the non-biomass fraction can be used for internal analyses. NOTE 4 14C method is not validated for the determination of the energy related biomass content. 7 Calculation Examples of method specific calculations are presented in the method specific Annexes A, B and C. When the biomass content by weight and biomass content by calorific value is to be determined by the 14C method, the values are calculated from the biogenic carbon content. Examples of this calculation are given in C.7.5. If the origin of the biogenic constituents is unknown, then a good estimation can be obtained by assuming that cellulose is the primary source of the biogenic constituents, as cellulose is the main product of the photosynthesis carbon cycle. SIST EN 15440:2011

is the Total Carbon content; % Biogenic carbon is the amount of carbon with biogenic origin; TCBx
is the biomass content, expressed as a percentage by TC.
8.2 Performance characteristics In accordance with EN ISO 17025 and the actual vision on the presentation of the performance characteristics as is shown in recent ISO standards, no demands on performance characteristics are present in this European Standard. External data for the calculation of the expanded uncertainty of measurements are presented in Annex F where recent results of round robin and validation studies are summarized. These values should be used in combination with individual laboratory performance characteristics and a desired coverage factor to get the overall uncertainty that is demanded by the customer. EXAMPLE Practical example of usage of the data from Annex F: A laboratory wants to determine the expanded uncertainty of measurement of their SDM method (by mass). The intra-laboratory reproducibility for the laboratory calculated from internal validations studies and control charts was determined to be 2,5 % (RSD). The round robin results from the QUOVADIS study (Table F.2.1) give a RSD value of 3,4 % (at 70 % level). u c,rel = ( 2,52+3,42) = 4,2 % U rel = 2 × u c,rel
= 8,4 % where u c,rel is the combined uncertainty of measurement and U rel is the expanded uncertainty of measurement using a coverage factor of 2 (~ 95 % confidence interval).
Determination of biomass content using the selective dissolution method A.1 Introduction This annex specifies the procedures for the determination of the biomass content expressed in percent by weight, by calorific value and by carbon content using selective dissolution. The selective dissolution method is based on the fact that biomass oxidizes significantly more quickly than non-biomass. A.2 Principle The selective dissolution method for the determination of the biomass content expressed in percent by weight involves the treatment with concentrated sulphuric acid topped with hydrogen peroxide. The biomass in the solid recovered fuel will selectively dissolve and the non-biomass will remain in the residue. For the determination of the biomass content expressed in percent by weight, the sample shall be weighed before and after selective dissolution. The biomass content by weight is corrected for the content of carbonates by measuring the ash content (according to EN 15403) before and after dissolution. Figure A.1 shows which steps are performed when determining the biomass content by percent in weight using the selective dissolution method. The determination of the biomass content by calorific value consists of two procedures. The first procedure determines the calorific values of the total sample and non-biomass fraction. The second procedure calculates the biomass content by energy content. Figure A.2 illustrates the principle by which the fraction specific calorific values shall be determined. Depending on the use of the results, the biomass content may be calculated in percent by net calorific value or by gross calorific value. Before this annex is applied, a choice shall be made whether the biomass fraction shall be determined by net calorific value or gross calorific value. All calorific values in the rest of this annex will then be expressed according to that choice. The determination of the biomass content by carbon content involves the determination of the TC content before and after the selective dissolution of the biomass fraction. The results are used for the calculations of the biomass content expressed in percentage by TC. The maximum relative error for the biomass content by TC is 0,4 % per 1,0 percent by weight of the ash fraction. Therefore, a correction for carbonate present in the ashes is made if the ash content in the original sample (as determined in this annex is larger than 10 % by weight on a dry basis. Figure A.3 shows which steps are performed when determining the biomass content by using the selective dissolution method for the determination of the biomass content in percent by TC. A.3 Symbols For the purposes of this annex, the following abbreviated terms apply. ASRF
ash content of SRF sample according to EN 15403; Cash
total carbon content of the ash fraction expressed as a percentage by weight; Cresidue total carbon content of the non-biomass fraction expressed as a percentage by weight; Ctot total carbon content of the total sample expressed as a percentage by weight; SIST EN 15440:2011

dry ash free mresidue-ash
mass of ash of dissolution residue (including filter), burned according to EN 15403, in g; mSRF
mass of dry SRF test portion used for dissolution, in g; mresidue
remaining dry mass (including filter) after the test portion has been dissolved, in g; qB
calorific value of the biomass fraction on a dry and ash-free basis, in MJ/kg; qNB
calorific value of the non-biomass fraction on a dry and ash-free basis, in MJ/kg; qresidue calorific value of the residue resulting from the dissolution test on a dry basis, in MJ/kg; qSRF
calorific value of the SRF on a dry basis sample, in MJ/kg; TC
total carbon; Bx
biomass content expressed as a percentage by weight; xNB
non-biomass expressed as a percentage by weight; calBx
biomass content expressed as a percentage by calorific value; calNBx non-biomass content expressed as a percentage by calorific value; TCBx biomass content expressed as a percentage by TC; residuex amount of dissolution residue, expressed as a percentage by weight. A.4 Reagents and materials Reagents and materials needed for performing the selective dissolution method are:  78 % (g/g) H2SO4 (laboratory quality);  35 % (g/g) H2O2 (laboratory quality);  glass fibre filter, ∅ 10 cm, GF 6 (this means that it is a filter which is equipped to block particles larger than 1µm); In case of high biomass content SRF a smaller diameter filter can be used.
 water of at least demineralized quality. A.5 Apparatus Apparatus needed for performing the selective dissolution method are:  Büchner funnel, ∅ 10 cm;  conical flask (500 ml);  desiccator; SIST EN 15440:2011

 cutting grinder or other grinding apparatus that can be used to reduce samples to < 1 mm;  fume cupboard;  pH measuring device;  scales accurate to 1 mg. A.6 Procedure for the determination of the biomass content expressed in percent by weight A.6.1 General This procedure specifies the determination of the biomass content expressed in percent by weight, using the selective dissolution method. Figure A.1 illustrates the principle by which the percentage by weight is determined.
Figure A.1 — Selective dissolution method for biomass content expressed in percent by weight A.6.2 Procedure Sample preparation in the field shall be conducted according to EN 15442 and EN 15443. Preparation of the test sample shall be conducted according to EN 15413. Perform the following steps for implementing the selective dissolution method: a) take two test portions of 5 g and a nominal top size of 1 mm according to EN 15413. Record the weight of the two test portions; b) determine the ash content of test portion A, ASRF according to EN 15403. When the biomass content expressed in percent by total carbon is to be determined (see A.8), the ash shall be retained; SIST EN 15440:2011

CEN/TS 15414-1 and cool in a desiccator; WARNING — For some types of solid recovered fuels there can be a risk of self-ignition when drying at 105 °C. d) weigh the dried test portion B with four digit precision. Record the weight (mSRF); e) place test portion B in an empty 500 ml flask; f) make sure the crucible is completely empty after emptying into the flask. If not, the weight before and after emptying shall be determined which enables the recalculation of mSRF; g) add 150 ml of 78 % (g/g) H2SO4 to the conical flask. Stir carefully, but thoroughly by hand. The sample has to be completely moistened with H2SO4. Place the (full) flask away in a fume cupboard for 16 h ± 2 h (cooling may be required); h) after 16 h ± 2 h, add 30 ml of 35 % (g/g) H2O2. Add slowly to control the reaction. Stir carefully, but thoroughly by hand. The sample has to be completely moistened with H2O2. Place the conical flask away in a fume cupboard for 5 h ± 1 h (cooling may be required); i) dry a glass fibre filter and record the weight of the glass fibre filter (mfilter); j) after 5 h ± 1 h, dilute the sample B with 300 ml of demineralised water and then filter it over a glass fibre filter in a Büchner funnel; k) remove the sulphuric acid by rinsing the residue with 6 doses of 50 ml demineralised water. Make sure the entire 50 ml demineralised water is removed before another dose is added or until the last filtrated volume has a pH of at least 3,0; l) dry the residue B together with the filter at 105 °C until a constant weight has been achieved; WARNING — For some types of solid recovered fuels there can be a risk of self-ignition when drying at 105°C. m) weigh the dried residue B together with the filter and record the weight (mresidue) with four digit precision; n) determine the remaining mass of the ash (mresidue-ash) of sample B according to EN 15403. A.6.3 Calculation of the results The results of the dissolution test and the Equations (A.1 and A.2) shall be used to calculate the biomass content, the ash content and the non-biomass content on a dry basis expressed as a percentage by weight. Use Equation (A.1) for the determination of the biomass content on a dry basis expressed as a percentage by weight:
0011001SRFSRFash-residueresidueB×+−−=Ammmx (A.1) Use Equation (A.2) for the calculation of the non-biomass content on a dry basis. SRFBNB100Axx−−= (A.2) SIST EN 15440:2011

The non biomass content on dry basis can now be calculated (according to Equation (A.2)): 2,41158,43100=−−=ΝΒx
A.7 Procedure for the determination of calorific value of the biomass and non-biomass fraction A.7.1 General This procedure specifies the determination of fraction specific calorific values of biomass and non-biomass. These calorific values can be expressed either as net calorific value or as gross calorific value. Determination of the biomass content of solid recovered fuels is based on the selective dissolution method. A.7.2 Procedure The determination of the biomass content by calorific value consists of two procedures. The first procedure determines the calorific values of the biomass and non-biomass fraction. The second procedure calculates the biomass content by energy content. Figure A.2 illustrates the principle by which the fraction specific calorific values shall be determined. SIST EN 15440:2011

Figure A.2 — Determination of calorific value of the biomass and non-biomass fraction Depending on the use of the results, the biomass content may be calculated in percent by net calorific value or by gross calorific value. Before this annex is applied, a choice shall be made whether the biomass fraction shall be determined by net calorific value or gross calorific value. All calorific values in the rest of this annex will then be expressed according to the choice. The calorific value and the ash content of both the sample and the residue shall be determined according to EN 15400 and EN 15403 respectively. With these values the fraction specific calorific values shall be calculated. For conversion of data from dry base to as received base or dry ash free base the equations in EN 15296 can be used. In order to determine fraction-specific calorific values the following steps shall be performed: a) take a sample according to EN 15442 and prepare the sample according to EN 15443 and/or
EN 15413; b) determine the calorific value and the ash content of the sample according to EN 15400; c) determine the non-biomass content of a test portion according to A.6; d) take a new test portion and follow steps c) to m) of the instructions in A.6.2. Take care that sufficient residue of the sample is obtained via selective dissolution to perform the next step. However, if an SIST EN 15440:2011

100/1residueNBresidueAqq−=
(A.5)
Calculate the ash-free fraction-specific calorific value of the biomass fraction using Equation (A.6). Use the values obtained from Equation (A.5): ()100/100/1100/SRF(d)NB(daf)(daf) NBNB(daf) SRF(daf) BAxqxqq−−×−=
(A.6) Calculation example
EXAMPLE In a dry SRF sample, following properties were found: qSRF(d) = 18 MJ/kg(d); ash content ASRF(d) = 8 %(d). In the Selective dissolution test the amount of residue, xNB(daf) was 40 % , ash content ANB = 10 % and qNB= 25 MJ/kg(d). We now have:
())((daf) B/25,13100/8100/401)100/10(1/25100/4018dafkgMJq=−−×−= The procedure for determining the biomass content in percent by calorific value consists of four steps: a) determine the biomass content, Bx, and non-biomass content, NBx, according to A.6.3; b) determine the fraction specific calorific values according to A.7; c) determine the biomass content in percent by calorific value; d) calculate the calorific content of biomass and non-biomass in the calorific value of the overall sample using Equations (A.7) and (A.8):
SRFBBcalBqqxx×=
(A.7)
calBcalNB100xx−=
(A.8)
Figure A.3 — Selective dissolution method for biomass content in percent by TC A.8.2 Procedure The following steps shall be performed for implementing the selective dissolution method for the determination of the biomass content in percent by TC: SIST EN 15440:2011

x100totresidueresidueashSRFTCB×+×−=CCCAx
(A.8)
NOTE In the calculations, it is assumed that there is no inorganic carbon in the biomass fraction. Also, it is assumed that in the selective dissolution test all inorganic carbon is lost i.e. there is no inorganic carbon in the dissolution residue.
100totresidueresidueTCB×−=CCxx
(A.9)
Depending on the quality of the ash, a deviation of up to 0,4 % per 1,0 % of ash content may be caused by carbonates present in the ash. SIST EN 15440:2011

Determination of biomass content using the manual sorting method B.1 Introduction In the manual sorting method, a sample of the solid recovered fuel is sorted by hand into sub-fractions, such as plastics, paper/cardboard, wood, vegetable, fruit, garden waste and inert matter. B.2 Principle The manual sorting method for the determination of the biomass content in percent by weight involves the separation of the components into a number of fractions which are either (mostly) biomass or (mostly) non-biomass. The manual sorting error is determined for the specific type of SRF with the selective dissolution method. This method is not applicable for solid recovered fuels with a maximum particle size smaller than
10 mm and/or SRF that is pelletized. B.3
Symbols For the purposes of this annex, the following symbols apply. Bx biomass content on a dry basis, expressed as a percentage by weight; NBBx biomass content in the sorted non-biomass fraction on a dry and ash-free basis, expressed as a percentage by weight; Bix content component i in the biomass category on a dry basis, expressed as a percentage by weight; inertix content component i in the ash matter category on a dry basis, expressed as a percentage by weight; NBix content component i in the non-biomass category on a dry basis, expressed as a percentage by weight; inertx inert content on a dry basis, expressed as a percentage by weight; Binertx inert content in the sorted biomass fraction on a dry basis, expressed as a percentage by weight; NBinertx inert content in the sorted non-biomass fraction on a dry and ash-free basis, expressed as a percentage by weight; NBx non-biomass content on a dry basis, expressed as a percentage by weight; BNBx non-biomass content of the sorted biomass fraction on a dry basis, expressed as a percentage by
weight; SIST EN 15440:2011
0B sorting precision of the sorted biomas
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