1、BSI Standards PublicationPlastics Recycled plastics Determination of selected marker compounds in food grade recycled polyethylene terephthalate (PET)PD CEN/TS 16861:2015National forewordThis Published Document is the UK implementation of CEN/TS 16861:2015.The UK participation in its preparation was
2、 entrusted to TechnicalCommittee PRI/89, Plastics recycling.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisions ofa contract. Users are responsible for its correct application. The
3、British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 88025 4ICS 13.030.50; 83.080.20 Compliance with a British Standard cannot confer immunity fromlegal obligations.This Published Document was published under the authority of theStandards Policy and Strategy Commi
4、ttee on 30 June 2015. Amendments/corrigenda issued since publicationDate Text affectedPUBLISHED DOCUMENTPD CEN/TS 16861:2015TECHNICAL SPECIFICATION SPCIFICATION TECHNIQUE TECHNISCHE SPEZIFIKATION CEN/TS 16861 June 2015 ICS 13.030.50; 83.080.20 English Version Plastics - Recycled plastics - Determina
5、tion of selected marker compounds in food grade recycled polyethylene terephthalate (PET) Plastiques - Plastiques recycls - Dtermination de compositions de traceurs slectionns dans les poly(trphtalate dthylne) (PET) recycls de qualit alimentaire Kunststoffe - Kunststoff-Rezyklate - Bestimmung von Ma
6、rkierungsstoffen in Polyethylenterephthalat (PET)-Rezyklaten fr die Lebensmittelindustrie This Technical Specification (CEN/TS) was approved by CEN on 19 April 2015 for provisional application. The period of validity of this CEN/TS is limited initially to three years. After two years the members of
7、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
8、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, Cz
9、ech 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.
10、EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR 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 worldwide for CEN national Members. Ref. No. CEN/TS 16861:20
11、15 EPD CEN/TS 16861:2015CEN/TS 16861:2015 (E) 2 Contents Page Introduction . 5 1 Scope 6 2 Normative references 6 3 Terms and definitions . 6 4 Symbols and abbreviations 8 5 Principle 8 6 Reagents . 8 6.1 Carrier gases for gas chromatography . 9 6.2 Solvent 9 6.3 Standard solutions 9 7 Apparatus . 9
12、 7.1 Cryogenic mill 9 7.2 Laboratory glassware 9 7.3 Headspace gas chromatograph-mass spectrometer . 9 7.4 Capillary column 9 7.5 Refrigerator and freezer 9 7.6 Sieves 10 7.7 Analytical balance . 10 8 Procedures . 10 8.1 Introduction 10 8.2 Sample conservation . 10 8.3 Grinding of the PET samples 10
13、 8.3.1 General 10 8.3.2 Initial preparation . 10 8.3.3 Cleaning of the cryogenic mill prior to use and in-between samples 10 8.3.4 Cryogenic milling of the samples 11 8.3.5 Sieving of ground samples . 11 8.4 Preparation of standard solutions . 11 8.4.1 General 11 8.4.2 Stock solution A 11 8.4.3 Stoc
14、k solution B 12 8.4.4 Spiking solution . 12 8.5 Blank determinations 13 8.6 Preparation of sample vials 13 8.7 Gas chromatographic analysis 13 8.7.1 General 13 8.7.2 Identification and quantification of analytes using the standard addition method 13 9 Interference 15 9.1 Interference during sampling
15、 and storage 15 9.2 Interference due to co-elution 15 10 Test report 15 Annex A (informative) Representative chromatograms 16 A.1 Total ion chromatogram of all six analytes . 16 A.2 Chromatograms of individual analytes in the selected ion monitoring mode 16 PD CEN/TS 16861:2015CEN/TS 16861:2015 (E)
16、3 Annex B (informative) Example of instrument settings . 18 B.1 General . 18 B.2 Headspace sampler conditions . 18 B.3 Gas chromatography - mass spectrometry (GC-MS) conditions 19 B.4 Specific ions for selected ion mode (SIM) 19 Annex C (informative) Performance characteristics 20 C.1 General . 20 C
17、.2 Limit of detection . 20 C.3 Limit of quantification . 20 C.4 Precision 21 C.5 Accuracy 21 C.6 Linearity 22 C.7 Validation results . 22 Bibliography 23 PD CEN/TS 16861:2015CEN/TS 16861:2015 (E) 4 Foreword This document (CEN/TS 16861:2015) has been prepared by Technical Committee CEN/TC 249 “Plasti
18、cs”, the secretariat of which is held by NBN. 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 Re
19、gulations, 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, Ire
20、land, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. PD CEN/TS 16861:2015CEN/TS 16861:2015 (E) 5 Introduction In addition to drivers such as the recycling targets in the EU wa
21、ste packaging Directive (94/62/EC) and the economic cost of landfill taxes, there is a strong demand for recycled food grade plastic products from packaging end-users who are concerned about their corporate image and promoting their environmental responsibilities. To ensure that recycling systems an
22、d plants used for recycling plastics from post-consumer waste for food contact use are fit for purpose, the EU Commission published Regulation (EC) 282/2008 in 27th March 2008 (Recycled plastic materials and articles intended to come into contact with foods). Two of the main purposes of Regulation (
23、EC) 282/2008 are to define the conditions under which a recycling process should be run and managed and how an application to EFSA (European Food Safety Authority) to have the process authorized can be made. Even when plastics materials and articles are produced using a recycling process which has b
24、een authorized by EFSA, it is essential that they comply with the applicable food contact regulations, such as the Plastics Regulation (EU) 10/2011. It can take a long time for validation to approve new recycling processes, and the “Challenge” test to demonstrate the effectiveness of recycling proce
25、sses, which is described in Regulation (EC) 282/2008 and ultimately required by EFSA, can be relatively expensive and time consuming. The analytical method presented in this Technical Specification represents a novel, cost effective and relatively quick quality assurance tool that would support new
26、process development and assist organisations to conform to the EC regulations on recycled plastics. Also, because of its flexibility with respect to sample geometry, and small scale nature, the method can also be used in an ad hoc way to assess the quality of a wide range of recycled PET samples and
27、 products, for example flake, pellets, and products such as bottles and trays. The chemical compounds (called Marker compounds) for which the method is validated fall into two categories: those that are representative of the PET plastic (e.g. residual monomers), and the common flavour compound limon
28、ene. This Technical Specification is intended to serve two main purposes: to provide an analytical method to enable recyclers and end users of recycled food grade poly(ethyleneterephthalate) (PET) to identify and quantify the level of specific chemical compounds. As such, it provides a means of prov
29、iding a cost-effective, comparative assessment of its quality in terms of the presence and level of these chemical contaminants; to provide a template for the development of analytical methods for the analysis of specific “marker compounds” in other types of recycled food contact materials and artic
30、les, for example high density polyethylene (HDPE). This Technical Specification is intended to complement, but not to replace in any way, the existing chemical analysis tests, such as the EFSA “Challenge” test, used to assess the efficiency of PET recycling processes for food grade products, or the
31、EU overall and specific migration tests on food grade PET materials and articles using food products and/or food simulants. It is not intended to be used as a pass or fail type method, but to enable changes in the level of specific chemical compounds to be detected. This information could then be us
32、ed in a number of ways, depending upon the exact nature of the samples analysed, such as contributing to the information needed to justify a re-examination of a recycling process using the EFSA “Challenge” test. This Technical Specification is based on FP7 Project SupercleanQ. PD CEN/TS 16861:2015CE
33、N/TS 16861:2015 (E) 6 1 Scope This Technical Specification specifies an analytical method for testing food grade, recycled polyethylene terephthalate (PET). This analytical method provides / is intended to be used as a quality control check. This test identifies and quantifies certain specified cont
34、aminants. Such contaminants are referred to as Marker Compounds. The analytical method is applicable for use on PET samples and products at all stages in the recycling process and will therefore be useful to recycling companies producing commercial, recycled PET for food contact materials and articl
35、es, and the manufacturers of such articles. This Technical Specification is without prejudice to any existing legislation. NOTE Marker compounds are known to originate from two sources: from the PET material itself (i.e. residual monomers, degradation products or reaction/breakdown products); from f
36、ood products that the PET has contacted during its “first use”. WARNING The use of this Technical Specification might involve hazardous materials, operations and equipment. Persons using this Technical Specification should be familiar with normal laboratory practise. This document does not purport t
37、o address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practises and to ensure compliance with any national regulatory conditions. IMPORTANT It is absolutely essential that tests conducted according to th
38、is Technical Specification be carried out by suitably trained staff. 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 reference
39、s, the latest edition of the referenced document (including any amendments) applies. CEN/TS 16011, Plastics - Recycled plastics - Sample preparation EN ISO 472, Plastics - Vocabulary (ISO 472) 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN ISO 472 an
40、d the following apply. 3.1 analyte substance to be determined Note 1 to entry: In the context of this standard analyte refers to the selected marker compounds (3.4) in the PET sample. 3.2 diagnostic ion selected fragment ion, molecular ion or other characteristic ion from the mass spectrum of the ta
41、rget compound, chosen to provide good specificity and sufficient sensitivity PD CEN/TS 16861:2015CEN/TS 16861:2015 (E) 7 3.3 laboratory sample sample or subsample(s) sent to or received by the laboratory Note 1 to entry: In the context of this standard laboratory sample refers to sample of recycled
42、PET, in the form or flakes or pellets, or recycled PET food grade products intended to be used for the laboratory tests and from which the test sample (3.9) will be removed. Note 2 to entry: When the laboratory sample is further prepared (reduced) by subdividing, cutting, sawing, coring, or by combi
43、nations of these operations, the result is the test sample. When no preparation of the laboratory sample is required, the laboratory sample is the test sample. A test portion is removed from the test sample for the performance of the test or for analysis. The laboratory sample is the final sample fr
44、om the point of view of sampling but it is the initial sample from the point of view of the laboratory. Note 3 to entry: Several laboratory samples may be prepared and sent to different laboratories or to the same laboratory for different purposes. When sent to the same laboratory, the set is genera
45、lly considered as a single laboratory sample and is documented as a single sample. 3.4 marker compound chemical compound that is a typical contaminant present in post-consumer food grade PET and is the type of species that an approved recycling process is expected to remove to a safe level Note 1 to
46、 entry: The marker compound can originate from either the PET itself or the food products that it has been in contact with during service. 3.5 recycled food grade PET recycled PET in the form of flake or pellets from an extruder that has been recycled from post-consumer food grade PET waste using a
47、recycling process that has passed a “Challenge” test and meets the requirements of the EU Regulation (EC) 282/2008 Note 1 to entry: Flake dimensions are typically 2 mm to 5 mm. 3.6 recycled food grade PET products PET products, such as bottles and trays, which are intended for food use and have been
48、 manufactured from recycled PET that meets the requirements of EU Regulation (EC) 282/2008 3.7 selected ion mode, SIM measuring the intensity of selected diagnostic ions only 3.8 standard solution solution of accurately known concentration, prepared using standard substances in one or several ways N
49、ote 1 to entry: In the context of this standard a standards solution is a solution containing a set of marker compounds (analytical standards) prepared at a known concentration. 3.9 test sample sample, prepared from the laboratory sample, from which test portions are removed for testing or analysis Note 1 to entry: In the context of this standard test sample refers to aliquot of cryogenically ground and sieved laboratory sample (3.3) which will be analysed for the marker compounds. PD CEN/TS 16861:2015CEN/TS 16861:2015 (E) 8 4 Symbols
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