1、September 2016 English price group 9No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 59.080.01!%ZP“2559645www.din.de
2、DIN EN ISO 17881-1Textiles Determination of certain flame retardants Part 1: Brominated flame retardants (ISO 17881-1:2016);English version EN ISO 17881-1:2016,English translation of DIN EN ISO 17881-1:2016-09Textilien Bestimmung einiger Flammschutzmittel Teil 1: Bromierte Flammschutzmittel (ISO 178
3、81-1:2016);Englische Fassung EN ISO 17881-1:2016,Englische bersetzung von DIN EN ISO 17881-1:2016-09Textiles Dtermination de certains retardateurs de flamme Partie 1: Retardateurs de flamme broms (ISO 17881-1:2016);Version anglaise EN ISO 17881-1:2016,Traduction anglaise de DIN EN ISO 17881-1:2016-0
4、9www.beuth.deDocument comprises 14 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.08.16 DIN EN ISO 17881-1:2016-09 2 A comma is used as the decimal marker. National foreword This document (EN ISO 17881-1:2016) has been prepare
5、d by Technical Committee ISO/TC 38 “Textiles” in collaboration with Technical Committee CEN/TC 248 “Textiles and textile products” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Tes
6、ting), Working Committee NA 062-05-12 AA Textilchemische Prfverfahren und Fasertrennung. EN 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 retardants EUROPEAN STANDARD
7、 NORME EUROPENNE EUROPISCHE NORM EN ISO 17881-1 February 2016 ICS 59.080.01 English Version Textiles - Determination of certain flame retardants - Part 1: Brominated flame retardants (ISO 17881-1:2016) Textiles - Dtermination de certains retardateurs de flamme - Partie 1: Retardateurs de flamme brom
8、s (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 members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for g
9、iving 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 o
10、fficial 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
11、 of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech 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, Spai
12、n, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide
13、 for CEN national Members. Ref. No. EN ISO 17881-1:2016 EForeword 41 Scope .52 Principle 53 Reagents 54 Apparatus .65 Procedure.65.1 Preparation of standard solutions . 65.1.1 Stock standard solution .65.1.2 Internal standard solution . 65.1.3 Working solution . 75.2 Preparation of test specimen 75.
14、3 Ultrasonic wave extraction . 75.4 Flame retardants determination . 76 Calculation 77 Test report .8Annex A (informative) Test parameters by GC-MS .Annex B (informative) Round Robin test 11Contents PageEN ISO 17881-1:2016 (E) DIN EN ISO 17881-1:2016-092European foreword .39European foreword This do
15、cument (EN ISO 17881-1:2016) has been prepared by Technical Committee 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
16、publication of an identical text or by endorsement, at the latest 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 CENEL
17、EC shall not be held responsible for identifying any or all such patent 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 Republi
18、c, 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 the United Kingdom. Endorse
19、ment notice The text of ISO 17881-1:2016 has been approved by CEN as EN ISO 17881-1:2016 without any modification. EN ISO 17881-1:2016 (E) DIN EN ISO 17881-1:2016-093 ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member b
20、odies). The work of preparing International 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 a
21、nd non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are d
22、escribed in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be 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 draw
23、n 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 identifying 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 t
24、he ISO list of patent declarations received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment
25、, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 38, Textiles.ISO 17881 consists of the following parts, under the general titl
26、e Textiles Determination of certain flame retardants: Part 1: Brominated flame retardants Part 2: Phosphorus flame retardantsEN ISO 17881-1:2016 (E) DIN EN ISO 17881-1:2016-094 WARNING This International Standard calls for the use of substances and/or procedures that may be injurious to health if ad
27、equate precautions 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 appropria
28、tely qualified and 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 extra
29、cted from textile specimen 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
30、. 2052-07-5.3.2 Dibromobiphenyl (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 (H
31、eptaBB), CAS no. 88700-06-5.3.8 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.EN ISO 17881-1:2016 (E) DIN EN ISO 17881-1:2016-095 3.12 Pe
32、ntabromodiphenylether (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 Hexabro
33、mocyclododecane (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 this
34、 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, 0,4
35、5 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 solutions
36、 may be available in a different solvent.5.1.2 Internal standard solutionPrepare 10 g/ml standard solution of decachlorobiphenyl in toluene.EN ISO 17881-1:2016 (E) DIN EN ISO 17881-1:2016-096 5.1.3 Working solutionPrepare an admixture working solution of 17 flame retardants in internal standard solu
37、tion (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 sample. Cut it into s
38、mall 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. Filter and transfer
39、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 evaporator device (4.3
40、). 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). The test paramete
41、rs 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 the linear detector
42、 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 specimen, in g/g. Cal
43、culate 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 blank solution, in g/ml;
44、V is the final volume of the specimen solution, in ml;m is the mass of the test specimen, in g.EN ISO 17881-1:2016 (E) DIN EN ISO 17881-1:2016-097 7 Test reportThe test report shall include the following information:a) a reference to this part of ISO 17881, i.e. ISO 17881-1:2016;b) all details neces
45、sary for identification of the sample tested;c) the content of each flame retardant;d) any deviation from the procedure specified.EN ISO 17881-1:2016 (E) DIN EN ISO 17881-1:2016-098 Annex A (informative) Test parameters by GC-MSA.1 Instrument parametersAs the instrumental equipment of the laboratori
46、es 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 equivalent;b) Temperature programme: 100 C for 2 min, 100 C to
47、 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) 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 ions/amu Detection limit(g/g)Target ion
