1、BSI Standards PublicationBS EN ISO 17881-1:2016Textiles Determination ofcertain flame retardantsPart 1: Brominated flame retardants (ISO17881-1:2016)BS EN ISO 17881-1:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO17881-1:2016.The UK participation in it
2、s preparation was entrusted to TechnicalCommittee TCI/80, Chemical testing of textiles.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for it
3、s correctapplication. The British Standards Institution 2016. Published by BSI StandardsLimited 2016ISBN 978 0 580 82633 7ICS 59.080.01Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and St
4、rategy Committee on 31 March 2016.Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORMEN ISO 17881-1 February 2016 ICS 59.080.01 English Version Textiles - Determination of certain flame retardants - Part 1: Brominated flame retardants (ISO 17881-1:2
5、016) Textiles - Dtermination de certains retardateurs de flamme - Partie 1: Retardateurs de flamme broms (ISO 17881-1:2016) Textilien - Bestimmung einiger Flammschutzmittel - Teil 1: Bromierte Flammschutzmittel (ISO 17881-1:2016) This European Standard was approved by CEN on 11 December 2015. CEN me
6、mbers 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 applica
7、tion 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 Manag
8、ement 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
9、, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix
10、 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 17881-1:2016 EBS EN ISO 17881-1:2016EN ISO 17881-1:2016 (E) 3 European foreword This document (EN ISO 17881-1:2016) has been prepared by Technical Commit
11、tee ISO/TC 38 “Textiles” in collaboration with Technical Committee CEN/TC 248 “Textiles and textile products” the secretariat of which is held by BSI. 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
12、by August 2016, and conflicting national standards shall be withdrawn at the latest by August 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 p
13、atent 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 Macedoni
14、a, 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. Endorsement notice The text of ISO 17881-1:2016 has been approved by CEN
15、as EN ISO 17881-1:2016 without any modification. BS EN ISO 17881-1:2016ISO 17881-1:2016(E)Foreword iv1 Scope . 12 Principle 13 Reagents 14 Apparatus . 25 Procedure. 25.1 Preparation of standard solutions . 25.1.1 Stock standard solution . 25.1.2 Internal standard solution . 25.1.3 Working solution .
16、 35.2 Preparation of test specimen 35.3 Ultrasonic wave extraction . 35.4 Flame retardants determination . 36 Calculation 37 Test report . 4Annex A (informative) Test parameters by GC-MS . 5Annex B (informative) Round Robin test . 7 ISO 2016 All rights reserved iiiContents PageBS EN ISO 17881-1:2016
17、ISO 17881-1:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a sub
18、ject 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 with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (I
19、EC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be
20、noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifyi
21、ng any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience
22、of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Suppl
23、ementary informationThe committee responsible for this document is ISO/TC 38, Textiles.ISO 17881 consists of the following parts, under the general title Textiles Determination of certain flame retardants: Part 1: Brominated flame retardants Part 2: Phosphorus flame retardantsiv ISO 2016 All rights
24、reservedBS EN ISO 17881-1:2016INTERNATIONAL STANDARD ISO 17881-1:2016(E)Textiles Determination of certain flame retardants Part 1: Brominated flame retardantsWARNING This International Standard calls for the use of substances and/or procedures that may be injurious to health if adequate precautions
25、are not taken. It refers only to technical suitability and does not absolve the user from legal obligations relating to health and safety at any stage. It has been assumed in the drafting of this International Standard that the execution of its provisions is entrusted to appropriately qualified and
26、experienced people.1 ScopeThis part of ISO 17881 specifies a test method for determining some brominated flame retardants in textiles by gas chromatography mass spectrometry (GC-MS).The method is applicable to all kinds of textile products.2 PrincipleThe flame retardants are extracted from textile s
27、pecimen by ultrasonic generator with toluene. The flame retardants in the specimen are identified by GC-MS and quantified by using internal standard method.3 ReagentsUnless otherwise specified, use only reagents of recognized analytical grade.3.1 Monobromobiphenyl (MonoBB), CAS no. 2052-07-5.3.2 Dib
28、romobiphenyl (DiBB), CAS no. 57422-77-2.3.3 Tribromobiphenyl (TriBB), CAS no. 59080-34-1.3.4 Tetrabromobiphenyl (TetraBB), CAS no. 60044-24-8.3.5 Pentabromo-1,1-biphenyl (PentaBB), CAS no. 59080-39-6.3.6 Hexabromobiphenyl (HexaBB), CAS no. 60044-26-0.3.7 Heptabromo-1,1-biphenyl (HeptaBB), CAS no. 88
29、700-06-5.3.8 Octabromobiphenyl (OctaBB), CAS no. 67889-00-3.3.9 Nonabromobiphenyl (NonaBB), CAS no. 69278-62-2.3.10 Decabromobiphenyl (DecaBB), CAS no. 13654-09-6.3.11 Tetrabromodiphenylether (TetraBDE), CAS no. 5436-43-1. ISO 2016 All rights reserved 1BS EN ISO 17881-1:2016ISO 17881-1:2016(E)3.12 P
30、entabromodiphenylether (PentaBDE), CAS no.32534-81-9.3.13 Hexabromodiphenylether (HexaBDE), CAS no. 207122-15-4.3.14 Heptabromodiphenylether (HeptaBDE), CAS no. 207122-16-5.3.15 Octabromodiphenylether (OctaBDE), CAS no. 337513-72-1.3.16 Decabromodiphenylether (DecaBDE), CAS no. 1163-19-5.3.17 Hexabr
31、omocyclododecane (HBCDD), CAS no. 25637-99-4.3.18 Decachlorobiphenyl, CAS no.2051-24-3, internal standard (IS).3.19 Toluene.NOTE Since brominated flame retardants have many isomers, this method might not cover all of them. Determination of the isomers of flame retardants in Clause 3 can refer to thi
32、s method according to the principle.4 Apparatus4.1 Gas chromatography mass spectrometry (GC-MS).4.2 Ultrasonic generator, with a frequency from 35 kHz to 45 kHz.4.3 Evaporator device, with water bath at 50 C.4.4 Brown glass vial, 40 ml with tight closure.4.5 Flask, 100 ml.4.6 Filtration membrane, 0,
33、45 m.4.7 Balance, an accuracy of 0,1 mg.5 Procedure5.1 Preparation of standard solutions5.1.1 Stock standard solutionPrepare 1 000 g/ml of stock standard solutions with individual flame retardant (3.1 to 3.17) and internal standard (3.18) in toluene (3.19).Some commercial reference material solution
34、s may be available in a different solvent.5.1.2 Internal standard solutionPrepare 10 g/ml standard solution of decachlorobiphenyl in toluene.2 ISO 2016 All rights reservedBS EN ISO 17881-1:2016ISO 17881-1:2016(E)5.1.3 Working solutionPrepare an admixture working solution of 17 flame retardants in in
35、ternal standard solution (5.1.2) and dilute it to a series of suitable concentrations depending on test needs. Select at least five dilutions of the calibration sets to create calibration curve and perform GC-MS analysis.5.2 Preparation of test specimenPrepare a representative test specimen of the s
36、ample. Cut it into small pieces and weigh (1,00 0,01) g of the pieces with a balance (4.7).5.3 Ultrasonic wave extractionPut the pieces in a vial with tight closure (4.4) and add 20 ml of toluene. Place the vial in an ultrasonic generator (4.2) and extract the pieces for 30 min at room temperature.
37、Filter and transfer the extract into 100 ml flask (4.5). Add 10 ml of toluene to the residue in the vial and place the vial in the ultrasonic generator to extract the residue for 15 min at room temperature. Filter and merge the extract into the flask (4.5).Evaporate the extract to near dryness by ev
38、aporator device (4.3). Add 2 ml of internal standard solution (5.1.2) to dissolve the residue and then filter by filtration membrane (4.6). The filtrate is ready for determination of flame retardants.5.4 Flame retardants determinationDetermine the flame retardants in the solution (5.3) by GC-MS (4.1
39、). The test parameters by GC-MS are given in Annex A as an example. Run a blank to control contamination.When the flame retardants level is very low, it is necessary to increase the mass of the pieces in order to reach at least three times the detection limit.When the flame retardant level is beyond
40、 the linear detector response range of the equipment, it is necessary to dilute the specimen liquid properly.6 CalculationQuantify the concentration of each flame retardant by using the calibration curve. The content of each flame retardant is expressed by the mass ratio of flame retardant to test s
41、pecimen, in g/g. Calculate the result by using Formula (1).XCC Vmii=()0(1)whereXiis the content of the flame retardant, i, in the textile specimen, in g/g;Ciis the concentration of the flame retardant, i, in the specimen solution, in g/ml;C0is the concentration of the flame retardant, i, in the blan
42、k solution, in g/ml;V is the final volume of the specimen solution, in ml;m is the mass of the test specimen, in g. ISO 2016 All rights reserved 3BS EN ISO 17881-1:2016ISO 17881-1:2016(E)7 Test reportThe test report shall include the following information:a) a reference to this part of ISO 17881, i.
43、e. ISO 17881-1:2016;b) all details necessary for identification of the sample tested;c) the content of each flame retardant;d) any deviation from the procedure specified.4 ISO 2016 All rights reservedBS EN ISO 17881-1:2016ISO 17881-1:2016(E)Annex A (informative) Test parameters by GC-MSA.1 Instrumen
44、t parametersAs the instrumental equipment of the laboratories may vary, no generally applicable parameters can be provided for chromatographic analyses. The following parameters have been found successfully.a) Capillary column: VF-5ht, length 15 m, inside diameter 0,25 mm,film thickness 0,1 m or equ
45、ivalent;b) Temperature programme: 100 C for 2 min, 100 C to 310 C (20 C/min), 310 C for 5 min;c) Injector temperature: 280 C;d) Transfer line temperature: 300 C;e) Carrier gas: Helium with a purity of no less than 99,999 % delivered at 1,5 ml/min;f) Ionization mode: EI;g) Ionization energy: 70 eV;h)
46、 Detection mode: Selected ion monitor detection;i) Injector system: Splitless, split at 1 min;j) Injector volume: 1 l.A.2 Typical ions and detection limitTypical ions and detection limit for flame retardants are shown in Table A.1.Table A.1 Typical ions and detection limitNo. Flame retardantTypical
47、ions/amu Detection limit(g/g)Target ion Target ion1 Monobromobiphenyl (MonoBB) 152 234, 232, 152 52 Dibromobiphenyl (DiBB) 152 312, 310, 152 53 Tribromobiphenyl (TriBB) 230 392, 390, 230 54 Tetrabromobiphenyl (TetraBB) 310 470, 310, 308 55 Pentabromo-1,1-biphenyl (PentaBB) 388 550, 390, 388 56 Hexab
48、romobiphenyl (HexaBB) 468 628, 468, 466 57 Heptabromo-1,1-biphenyl (HeptaBB) 546 705, 546, 544 108 Octabromobiphenyl (OctaBB) 544 785, 546, 544 109 Nonabromobiphenyl (NonaBB) 705 864, 705, 703 10 ISO 2016 All rights reserved 5BS EN ISO 17881-1:2016ISO 17881-1:2016(E)No. Flame retardantTypical ions/a
49、mu Detection limit(g/g)Target ion Target ion10 Decabromobiphenyl (DecaBB) 783 944, 783, 781 1011 Tetrabromodiphenylether (TetraBDE) 326 488, 486, 326 512 Pentabromodiphenylether (PentaBDE) 404 564, 406, 404 513 Hexabromodiphenylether (HexaBDE) 484 643, 484, 482 514 Heptabromodiphenylether(HeptaBDE) 562 722, 562, 456 515 Octabromodiphenylether (OctaBDE) 642 801, 642, 639 516 Decabromodiphenylether (DecaBDE) 799 959, 799, 797 1017 Hexabromocyclododecane (HBCDD) 157 319, 239, 157 1018 Decachlorobiphenyl (IS) 498 498
