SIST EN 16640:2017

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.UDGLRRJOMLþQRPHWRGRBiobasierte Produkte - Gehalt an biobasiertem Kohlenstoff - Bestimmung des Gehalts an biobasiertem Kohlenstoff mittels RadiokarbonmethodeProduits biosourcés - Teneur en carbone biosourcé - Détermination de la teneur en carbone biosourcé par la méthode au radiocarboneBio-based products - Bio-based carbon content - Determination of the bio-based carbon content using the radiocarbon method71.040.40Kemijska analizaChemical analysis13.020.55Biološki izdelkiBiobased productsICS:Ta slovenski standard je istoveten z:EN 16640:2017SIST EN 16640:2017en,fr,de01-junij-2017SIST EN 16640:2017SLOVENSKI
STANDARDSIST-TS CEN/TS 16640:20141DGRPHãþD

EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16640
February
t r s y
vEnglish Version
Bioæbased products æ Bioæbased carbon content æ Determination of the bioæbased carbon content using the radiocarbon method Produits biosourcés æ Teneur en carbone biosourcé æ Détermination de la teneur en carbone biosourcé par la méthode au radiocarbone
Biobasierte Produkte æ Gehalt an biobasiertem Kohlenstoff æ Bestimmung des Gehalts an biobasiertem Kohlenstoff mittels Radiokarbonmethode This European Standard was approved by CEN on
v December
t r s xä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
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t r s y CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x x v rã t r s y ESIST EN 16640:2017

Procedures for sampling of products . 15 A.1 General . 15 Table A.1. — Sampling procedures . 15 Annex B (normative)
Procedure for the conversion of the carbon present in the sample to a suitable sample for 14C determination . 16 B.1 General . 16 B.2 Sample preparation . 16 Table B.1— Sample preparations . 16 B.3 Preparation for 14C measurement . 16 B.3.1 General . 16 B.3.2 Reagents and materials . 17 B.4 Combustion of the sample . 17 SIST EN 16640:2017

Method A - Liquid scintillation-counter method (LSC) . 21 C.1 General . 21 C.2 Principle . 21 C.3 Reagents and materials . 21 C.4 Apparatus . 21 C.5 Procedure . 22 C.5.1 General . 22 C.5.2 Benzene conversion . 22 C.5.3 Direct absorption of the CO2 in a carbamate solution . 22 C.5.4 Measurement . 22 C.5.5 Blank correction . 23 C.6 Calculation of the results . 23 Annex D (informative)
Method C - Beta-ionization (BI) . 24 D.1 General . 24 D.2 Principle . 24 D.3 Reagents and materials . 24 D.4 Apparatus . 25 D.5 Procedure . 25 D.6 Calculation of the results . 26 Annex E (normative)
Method B - Accelerator Mass Spectrometry (AMS) . 27 E.1 General . 27 E.2 Principle . 25 E.3 Reagents and materials . 27 E.4 Apparatus . 27 E.5 Procedure . 27 E.6 Calculation of the results . 28 Annex F (informative)
Performance characteristics . 29 Table F.1 — description of sample types . 29 Table F.2 — Performance data for 14C methods . 30 Bibliography . 31 SIST EN 16640:2017

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. SIST EN 16640:2017

(BI) - Low background laboratory - Gas purification device 8 h to 24 h 0,2 % to 5 % Low For the 14C LSC measurement a Low Level Counter shall 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. When using method A (LSC), samples with low bio-based carbon content (<10 %) can only be measured with sufficient precision using the benzene conversion procedure or, if applicable, direct LSC measurement, as described in Annex B. NOTE 2 At this moment compact new AMS equipment has become available. In a number of cases, no graphite conversion is required anymore. SIST EN 16640:2017

NOTE The pMC value of NIST SRM 4990 is set at 100, being equivalent to a 14C activity of 13,56 dpm/g C. 7.3.1.2 14C content determined by Method B (AMS) Calculate the bio-based carbon content by dry mass, xB, expressed as a percentage, using Formula (2): TCTCB()()100100pMCspMCsxxxREFREF===(2)=where=xTC is the total carbon content, expressed as a percentage, of the total dry mass of the sample; pMC(s) is the measured value, expressed in pMC, of the sample; SIST EN 16640:2017

7.3.2 Calculation of the bio-based carbon content xTCB as a fraction of TC Calculate the bio-based carbon content as a fraction of the total carbon content,TCBx, expressed as a percentage, using Formula (3): TCBBTC100xxx=×=(3)=where=xB is the bio-based carbon content by dry mass, expressed as a percentage; xTC is the total carbon content, expressed as a percentage, of the sample. 7.3.3 Examples EXAMPLE 1 Measurement according to Method A Sample made from pure wood (REF = 112 pMC, xTC = 48,0 %) Dry mass of sample: m = 1,010 g 14C activity = 7,34 dpm B7,3410047,8%11213,561,01100x=×=××=TCB47,810099,6%48,0x=×==EXAMPLE=2=Meas×rement=according=to=Method=B=Sample=made=from=xxx=(REF===112=pMC,=xTC = 52,0 %) NaOH solution: 1 M pMC(s) (Measured 14C value) = 61,7 pMC B61,71005228,6%112100x===TCB28,610055,0%52,0x=×==EXAMPLE=3=Calc×lation=of=bio-based=carbon=content=as=a=fraction=of=TC=P×re=bio-based=polymer=material=Sample=made=from=PLA=material:=(xTC===50,0=%;=xB===50=%)=SIST EN 16640:2017

Procedures for sampling of products A.1
General If available, product-sampling procedures for the determination of the total carbon content shall be used. If no such standard is available, a list of most suitable standards is given in Table A.1 as guidance. In the case of solid products, the sampling procedures mentioned in Table A.1 shall be used. If the procedure for solid product sampling is not available, then EN 15442 [8] or EN 15443 [9] shall be used. Table A.1. — Sampling procedures Products Sampling methods Solid products
Plastics, polymers ISO 10210 [10] Fuels EN 14780 [11], EN 14778 [12], EN 15442 [13], EN 15443 [14] ISO 13909 [15], ISO/NP 18135 [16], ISO 18283 [17], ISO 20904 [19], ASTM D7026–13 [20], Ceramics, glass, concrete, cement, construction materials / waste ASTM C172/C172M-10 [21], ASTM C224–78 [22], ASTM C322–09 [23], ASTM C1704/C1704M-09A [24], ASTM D3665–12 [25] Rubber ISO 1795 [26], ASTM D1485–07 [27] (2011), ASTM D6085–97 [28] (2011) Paper EN ISO 186 [29], EN 27213 [30], ASTM D2915–10 [31] Liquid products
Solvents ASTM D 268–01 [33] (2012), ASTM D802–02 [34] (2013), ASTM D3437–11 [35] Fuels ASTM D4057–12 [36], EN ISO 3170 [37], ASTM D4177–95 [38], EN ISO 3171 [39], ASTM D1265–11 [40], EN ISO 4257 [41], ISO 8943 [42], ASTM D233–12 [43], Gaseous products EN ISO 13833 [2] ISO 10715 [44] ASTM D7459–08 [45] Other suitable procedures EN ISO 15528 [46], ASTM D460–91 [47], ASTM D6866–12 [4], ASTM D7455–08 [48], ASTM D7718–11 [49], ASTM E300–03 [50] EPA 340/1–91–010 [51] ISO 5555:2001 [58] SIST EN 16640:2017

Procedure for the conversion of the carbon present in the sample to a suitable sample for 14C determination B.1 General In this annex, all steps are described to prepare samples for 14C determinations. In this way, a laboratory that is not equipped for 14C analysis can prepare their samples for distribution to laboratories that are equipped for 14C analysis. For the determination of the 14C content, the carbon that is present in the sample has to be converted to CO2. The conversion is done by combustion in oxygen. If necessary, a combustion aid can be used to ensure complete oxidation of the carbon to CO2. For a number of liquid samples, no conversion to CO2 is needed and direct measurement of the 14C content can be performed using LSC. B.2 Sample preparation For sample preparation procedures the following standards can be used: Table B.1— Sample preparations Products Sample preparation methods Solid products ISO 1928 [52], EN ISO 21068-2 [53], EN 15400, EN 15440 [1], CEN/TS 16137 [3], ASTM D6866 [4] Liquid products ASTM D6866 [4], ASTM D7455 [55], ASTM D5291 [56] Gaseous products EN ISO 13833 [2], ASTM D6866 [4] B.3 Preparation for 14C measurement B.3.1 General The 14C content of a bio-based product is determined on the CO2 produced by the sample combustion. For the conversion of the sample to CO2, used for the determination of the 14C content, the following three methods are allowed: — combustion in a calorimetric bomb; — combustion in a tube furnace; — combustion in a laboratory scale combustion apparatus. For gaseous samples, combustion in a calorimetric bomb is not applicable. Conversion of gaseous hydrocarbons to CO2 can be done at temperatures from 600 °C, using a suitable catalyst and absorption of the CO2 in a NaOH solution as described in B.3.2. SIST EN 16640:2017
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