1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS ISO 12418-2:2012Plastics Post-consumer poly(ethylene terephthalate) (PET) bottle recyclatesPart 2: Preparation of test specimens and determination of propertiesBS ISO 12418-2:
2、2012 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 12418-2:2012. The UK participation in its preparation was entrusted to T e c h n i c a l Committee PRI/82, Thermoplastic materials.A list of organizations represented on this committee can be obtained on requ
3、est to its secretary.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2012Published by BSI Standards Limited 2012ISBN 978 0 580 66137 2 ICS 83.080.20 Compliance with a British
4、 Standard cannot confer immunity from legal obligations.This British Standard was published under the authority of the Standards Policy and Strategy Committee on 30 September 2012.Amendments issued since publicationDate T e x t a f f e c t e dBS ISO 12418-2:2012 ISO 2012Plastics Post-consumer poly(e
5、thylene terephthalate) (PET) bottle recyclates Part 2: Preparation of test specimens and determination of propertiesPlastiques Recyclats de bouteilles en poly(trphtalate dthylne) (PET) post-consommation Partie 2: Prparation des prouvettes et dtermination des propritsINTERNATIONAL STANDARDISO12418-2F
6、irst edition2012-09-01Reference numberISO 12418-2:2012(E)BS ISO 12418-2:2012ISO 12418-2:2012(E)ii ISO 2012 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2012All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, e
7、lectronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.or
8、gWeb www.iso.orgPublished in SwitzerlandBS ISO 12418-2:2012ISO 12418-2:2012(E) ISO 2012 All rights reserved iiiContents PageForeword iv1 Scope 12 Normative references . 13 Terms and definitions . 14 Characterization of PET recyclates 14.1 Classification of characteristics 14.2 Test methods 1Annex A
9、(normative) Method for the determination of impurities in PET flakes . 3Annex B (normative) Method for the determination of the bulk density of PET flakes . 5Annex C (informative) Method for the determination of the melt volume-flow rate (MVR) of PET recyclates . 7Annex D (informative) Potentiometri
10、c method for the determination of the residual alkalinity of PET recyclates . 9Bibliography . 11BS ISO 12418-2:2012ISO 12418-2:2012(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Int
11、ernational Standards is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison w
12、ith ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.The main task of technica
13、l committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote.Attention is drawn to
14、the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights.ISO 12418-2 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 9, Thermoplastic materials.ISO 12418 co
15、nsists of the following parts, under the general title Plastics Post-consumer poly(ethylene terephthalate) (PET) bottle recyclates: Part 1: Designation system and basis for specifications Part 2: Preparation of test specimens and determination of propertiesiv ISO 2012 All rights reservedBS ISO 12418
16、-2:2012INTERNATIONAL STANDARD ISO 12418-2:2012(E)Plastics Post-consumer poly(ethylene terephthalate) (PET) bottle recyclates Part 2: Preparation of test specimens and determination of properties1 ScopeThis part of ISO 12418 specifies the test methods to be used in determining the properties of post-
17、consumer poly(ethylene terephthalate) (PET) bottle recyclates.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (
18、including any amendments) applies.ISO 472, Plastics VocabularyISO 1628-1, Plastics Determination of the viscosity of polymers in dilute solution using capillary viscometers Part 1: General principlesISO 1628-5, Plastics Determination of the viscosity of polymers in dilute solution using capillary vi
19、scometers Part 5: Thermoplastic polyester (TP) homopolymers and copolymersISO 15270, Plastics Guidelines for the recovery and recycling of plastics wasteISO 15512:2008, Plastics Determination of water contentEN 15348:2007, Plastics Recycled plastics Characterization of poly(ethylene terephthalate) (
20、PET) recyclates3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 472 and ISO 15270 apply.4 Characterization of PET recyclates4.1 Classification of characteristicsThe characteristics of PET recyclates are classified into two types, given in Table 1, as f
21、ollows: those which are required for all recyclates (i.e. mandatory characteristics); customer specifications (these are optional).4.2 Test methodsThe characteristics shall be determined using the test methods given in Table 1. A certificate of analysis, including the test results for each batch of
22、recyclate, the sampling method and the number of replicates, shall be provided by the supplier to the purchaser on request.NOTE The sampling method and the number of replicates are important in determining the quality of the material. Quality levels can vary within the batch and from batch to batch,
23、 depending on the source of the recyclate. ISO 2012 All rights reserved 1BS ISO 12418-2:2012ISO 12418-2:2012(E)Table 1 Characterization of PET recyclatesCharacteristics Unit Test method NotesMandatory itemsForm Visual examination Flakes, pellets or powderColour Visual examination Natural or coloured
24、Maximum flake size mm Determined by the size of the screen in the grinderMaximum pellet size mm Determined by the die opening of the pelletizer and measured by ruler or callipersIntrinsic viscosity (IV) dl/g ISO 1628-5 in combination with ISO 1628-1 (including its Amendment ISO 1628-1:2009/Amd 1)Sol
25、vent shall be a mixture of phenol and 1,1,2,2-tetrachloroethane (6:4)Contamination due to labels and other visible contaminantsmg/kg Annex A Only for flakesContamination due to poly(vinyl chloride)mg/kg Annex A Only for flakesContamination due to poly-olefins, and including adhesivemg/kg Annex A Onl
26、y for flakesWater content % ISO 15512:2008, method B Bulk density kg/m3Annex B Optional itemsMelt volume-flow rate (MVR) cm3/10 min Annex C Alkalinity pH Annex D Only for flakesFilterability 10 MPa/h/cm2EN 15348:2007, Annex F Other tests may be carried out by agreement between the purchaser and the
27、supplier. If they are, the results of such tests shall be reported.2 ISO 2012 All rights reservedBS ISO 12418-2:2012ISO 12418-2:2012(E)Annex A (normative) Method for the determination of impurities in PET flakesA.1 GeneralThis annex specifies a method for the determination of the content of the foll
28、owing impurities in flakes of PET recyclates: pieces of label and other visible contaminants; poly (vinyl chloride) (PVC); polyolefins (POs), and including adhesive.A.2 PrincipleA weighed test portion of the recyclate is spread evenly over the bottom of a shallow tray.The pieces of label and other v
29、isible contaminants are picked out using tweezers and weighed. The test portion, still in the tray, is then placed in a forced air circulation oven at 220 C for 1 h.During this heat treatment, the PVC in the test portion becomes discoloured and can be detected visually. The polyolefins in the test p
30、ortion melt and turn yellow. The adhesive is also yellowed and might be indistinguishable from the polyolefins.A.3 ApparatusA.3.1 Oven, with forced air circulation, capable of being maintained at 220 C.A.3.2 Technical balance, capable of weighing to the nearest 0,1 g.A.3.3 Analytical balance, capabl
31、e of weighing to the nearest 0,000 1 g.A.3.4 Spatula, made of wood or metal.A.3.5 Tweezers.A.3.6 Tray, made of aluminium or enamelled ironware, with a bottom of surface area not less than 0,05 m2.A.4 ProcedureWeigh out, to the nearest 0,1 g, approximately 100 g of flakes and record the mass (m0). Sp
32、read the flakes evenly over the bottom of the metal tray.Stir the flakes slowly in the tray with a spatula and pick out the pieces of label and other visible contaminants using tweezers. Continue this procedure for not less than 30 min. Weigh the pieces of label and other visible contaminants picked
33、 out (m1), using an analytical balance. ISO 2012 All rights reserved 3BS ISO 12418-2:2012ISO 12418-2:2012(E)Put the tray containing the remaining material into an oven, preheated to 220 C, and leave it at that temperature for 1 h. Remove the tray, allow to cool and inspect the material for not less
34、than 30 min, as follows:a) Pick out the black carbonized particles (PVC). Weigh the particles picked out (m2), using an analytical balance.b) Pick out the yellowish particles (POs and adhesive). If they are stuck to PET flakes, separate them. Weigh the particles picked out (m3), using an analytical
35、balance.A.5 Expression of resultsA.5.1 The content of label and other visible contaminants, expressed in mg/kg, is given by the following formula:Content of label and other visible contaminants =mm16010(A.1)wherem1is the mass of label and other visible contaminants, in g;m0is the initial mass of the
36、 test portion, in g.A.5.2 The PVC content, expressed in mg/kg, is given by the following formula:PVC content =mm26010(A.2)wherem2is the mass of the discoloured (black) particles, in g;m0is the initial mass of the test portion, in g.A.5.3 The PO content (which will include any adhesive present), expr
37、essed in mg/kg, is given by the following formula:PO content =mm36010(A.3)wherem3is the mass of the yellowish particles, in g;m0is the initial mass of the test portion, in g.A.6 Test reportThe test report shall include the following information:a) a reference to this part of ISO 12418 (ISO 12418-2);
38、b) all details necessary for identification of the sample tested;c) the results of the test;d) details of any additional operations carried out or changes made in the procedure;e) the date of the test.4 ISO 2012 All rights reservedBS ISO 12418-2:2012ISO 12418-2:2012(E)Annex B (normative) Method for
39、the determination of the bulk density of PET flakesB.1 PrincipleA container of known volume is weighed and then filled with PET flakes up to the brim and reweighed. The bulk density is calculated from the container volume and the mass of the PET flakes.B.2 ApparatusB.2.1 Container, approximately 120
40、 mm in diameter and approximately 150 mm in depth, with a smooth brim.B.2.1 Ruler, to remove sample material protruding above the brim of the container.B.2.1 Balance, capable of weighing to the nearest 0,1 g.B.3 ProcedureTake a sufficient amount of sample to allow three determinations to be carried
41、out.Weigh the container (mc1) to the nearest 0,1 g.Using a suitable scoop, fill the container until it overflows. Tap the brim of the container three times and level the contents across the brim of the container using a ruler. Weigh the filled container (mc2) to the nearest 0,1 g.Repeat the above pr
42、ocedure twice to give three results.B.4 CalculationCalculate the bulk density from the following formula:bcc=mmV21310wherebis the bulk density, in kg/m3;mc1is the mass of the container, in g;mc2is the mass of the test portion and container, in g;V is the volume of the container, in cm3.B.5 Test repo
43、rtThe test report shall include the following information:a) a reference to this part of ISO 12418 (ISO 12418-2);b) all details necessary for identification of the sample tested; ISO 2012 All rights reserved 5BS ISO 12418-2:2012ISO 12418-2:2012(E)c) the results of the test (the three individual resu
44、lts plus their mean);d) details of any additional operations carried out or changes made in the procedure;e) the date of the test.6 ISO 2012 All rights reservedBS ISO 12418-2:2012ISO 12418-2:2012(E)Annex C (informative) Method for the determination of the melt volume-flow rate (MVR) of PET recyclate
45、sC.1 GeneralThis annex specifies a method for the determination of the melt volume-flow rate (MVR) of PET recyclates in accordance with ISO 1133-1 and ISO 1133-2.C.2 Drying conditionsDry a test sample of PET recyclate at 160 C for 402+h in a circulating-air oven, prior to preforming a compacted char
46、ge by compression.NOTE Because PET is hygroscopic, its viscosity decreases rapidly due to hydrolysis if the material is allowed to absorb moisture. The test sample is therefore dried prior to testing in order to improve the comparability of test results.C.3 Preforming for flakesWhen flakes of PET re
47、cyclate are used, prepare a preformed compacted charge in accordance with Annex C of ISO 1133-1:2011, using the following conditions:a) cylinder temperature: 240 C to 242 C;b) mass of sample placed in cylinder: 6 g to 8 g;c) load on piston: 1,5 kN;d) loading time: 2 min under vacuum.C.4 Size of dieA
48、 half size die of length 4,000 mm 0,025 mm and bore diameter 1,050 mm 0,005 mm (see ISO 1133-1 and ISO 1133-2) shall normally be used. If testing materials using this die gives a melt volume-flow rate of less than 5 cm3/10 min, the standard die 8,000 mm 0,025 mm in length and having a bore of nomina
49、l diameter 2,095 mm should preferably be used.C.5 Test temperatureA test temperature of 280 C shall be used.C.6 Size of test sampleA test sample of mass 6 g to 10 g shall be used.C.7 Nominal load on pistonThe nominal load on the piston shall be 5 kg. ISO 2012 All rights reserved 7BS ISO 12418-2:2012ISO 12418-2:2012(E)C.8 Charging the cylinderIntroduce the dried test sample into the cylinder immediately after it has been taken out of the oven in order to avoid moisture regain. Durin
