20082, 1418 BS ENISO 17881-22016 TIES (Se) en <6 > QQ Mem Amey eme~ (mex a POF | mR 16 1 REE: 216-06-20250452 1 SRR: S801 RTF: 1000 | LAMAR 1m AE > mo eP DB Intpstwwvn.doe88,comp-£048838856125.Ntml 1820.08.23, 1418 BSENISO 17681-22016 HEE < 16> QQ (hw Ame 2a ~ BS EN ISO 17881-2:2016 i Z BSI Standards Publication Textiles — Determination of certain flame retardants Part 2: Phosphorus flame retardants (ISO 17881-2:2016) bsi. . making excellence Shavit’ a Aa tps Awww. docB8.conyp.8048898956126.html20.08.23, 14:18 <6 > BS EN ISO 17881-2:2016 Intpstwwvn.doe88,comp-£048838856125.Ntml BS ENISO 17881-22016 HS QQ (hme Awe - 2a ~ BRITISH STANDARD ‘National foreword ‘This British Standard isthe UK implementation of EN ISO. 17881-2:2016, ‘The UK participation in its preparation was entrusted to Technical Committee TCU80, Chemical testing of textiles. {lst of organizations represented on this committee can be ‘obtained on request 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 2016. Published by BSI Standards Limited 2016 ISBN 978 0 580 82634 4 ics 59,080.01 Compliance with a British Standard cannot confer immunity from legal obligations. This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 March 2016, “Amendments issued since publication Date Text affected > oP DB 3820.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hem Awme~ 2a ~ Q a EUROPEAN STANDARD EN ISO 17881-2 NORME EUROPEENNE EUROPAISCHE NORM February 2016 1c359.080.01 English Version Textiles - Determination of certain flame retardants - Part 2: Phosphorus flame retardants (ISO 17881-2:2016) ‘Texts - Détermination de certains etardateuts de ‘eaten - Bestimmung einige Pannschutznitel ‘nme Farle 2 Retardaters defame phosphors Tell: Phosphororganisehe lanmschutamtel (150 (so 17881-22016), iyuo1-220%0), “This European Standard wae approved by CEN on 11 Decembor 2015. ‘CEN members are bound to comply withthe CEN/CENELECInteral Regultions which stipulate the conditions for ving this European Standard the status o national standard witout any alteration Up-to-date sts and ibiograpical references neering sich ational stanartemsybe obtained on application tothe (EN-CENELEC Management Centre ott anyCEX “This European Standard cxstsin tre official versions (English, French, tralation ander the responsi CEN member nto so lansage nd oie the CEN-CEN an) Aversion nay other language made by Management EN menbersare the national standards boes of Austria, Belgium, Bulgaria. Croatia, Cypres, Czech Republic Denmark. Estnla, Finland, Former Tuosar Republic of Macedonia, Franc, Germans, Greer, Hangar. ela rel, Maly Lats, Lith, [Lunembourg. Maka, Netherlands, Wor. Pound, Portgal Reman Sovak, oven, sai, sweden, Sizer, Turkey and United Kingdon COMITE FUROPEEN DE-NORMALISATION ‘CEN-CENELEC Management Centre: Avenue Marnx 17, B-1000 Brussels {©BMCEK_ Alapistesoatonn anya andy ay mene red eo. 180 I7R-2:2016€ Se a Aa RBA, DH MESSY ~ SUAS, ERE, SHIR, LET, BemIORE! -ntpswwn.doe88,comp-£048838856125.Ntml ane20.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hem Awme~ 2a ~ BS EN ISO 17881-2:2016 EN 1S0 17881-2:2016 (E) European foreword ‘This document (ENISO 17881-22016) has been prepared by Technical Committee ISO/TC38 “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, atthe latest by August 2016, and conflicting national standards shall bbe withdrawn atthe 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 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 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 the United Kingdom, Endorsement no! e ‘The text of 1S0 17881-2:2016 has been approved by CEN as EN ISO 17881-2:2016 without any modification. > ep wD Intpstwwvn.doe88,comp-£048838856125.Ntml 51820.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hem Awme~ 2a ~ ISO 17881-2:2016(E) Contents Page Foreword wv 1 Scope 1 2 Principle. 4 3 Reagents cd 4 Apparatus 1 5 Procedure 2 5.1 Preparation of standard solutions 2 SiLL_ Stock standard solution 2 5.1.2 Working solution 2 52 Preparation of test specimen 2 53. Ultrasonic wave extraction 2 54 Flame retardants determination iz 6 Calculation 3 7 Test report. 3 Annex A (Informative) Test parameters by HPLC-MS/MS 4 Annex B (informative) Round Robin test. 6 & Se (© 190 2016 A rights reserved Si a Intpstwwvn.doe88,comp-£048838856125.Ntml 5820.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hw Ame 2a ~ Q 180 17881-2:2016(E) Foreword 150 (the International Organization for Standardization) isa worldwide Federation of national standards bodies (ISO member bodies}. The work of preparing International Standards is normally carried cut through 1S0 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 with 1SO, also take part in the work. 150 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of lectrotechnical standardization, ‘The procedures used to develop this document and those intended for its further maintenance are deseribed 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 ofthe ISO/IEC Directives, Part2 (see wwwsuiso.org/airectives), ‘Attention is dravin to the possibilty that some of the elements ofthis document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Detalls of Any patent rights identified during the development of the document will be inthe Introduction and/or ‘on the [80 list of patent declarations received (see wwwriso.org/patent}. ‘Any trade name used in this dacument fs 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, as well as information about 1S0's adherence to the WTO principles in the Technical Barriers to Trade (TT) soe the following URL: Foreword - Supplementary information ‘The committee responsible for this document is ISO/TC 38, Textiles. ISO 17881 consists ofthe following parts, under the general ttle Texvles — Determination of certain flame retardants: = Pare 1: Brominated flame retardants — Part 2: Phosphorus flame retardants w (0150 2016- rs eer a REBAR, RAMS CE UC, GSE, RAMEN, LNT, Ren! Fines -ntpswwn.doe88,comp-£048838856125.Ntml 1820.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hw Ame 2a ~ Q BS EN 150 17881-2:2016 INTERNATIONAL STANDARD. ISO 17881-2:2016(E) Textiles — Determination of certain flame retardants — Part 2: Phosphorus flame retardants WARNING — This International Standard calls for the use of substances and/or procedures that may be injurious to health ifadequate 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. Ithas been assumed in the drafting of this International Standard that the execution Of its provisions is entrusted to appropriately qualified and experienced people. 1 Scope This part of ISO 17881 specifies a test method for determining some phosphorous flame retardants in textiles by high performance liquid chromatography ~ tandem mass spectrometry (HPLC-MS/MS). ‘The method is applicable to all kinds of textile products. NOTE Fortes (I-aziritinyl] phosphineaside (TEPA), only unbonded TEPA is extractable, 2. Principle ‘The flame retardants are extracted from textile specimen by ultrasonic generator with acetone, The flame retardants in the specimen are identified and quantified by HPLC-MS/MS, 3. Reagents Unless otherwise specified use only reagents of recognized analytical grade, 3A Tris (2,3-dibromopropyl) phasphate (TRIS), CAS no, 126-72-7. 3.2 Tris (1-aziridiny!) phosphineoxide (TEPA), CAS no, 545-95-1 33. Tris (2-chloroethy!) phosphate (TCEP), CAS no, 115-96-8 3A Acetone. 3.5 Acetonitrile (ACN). 3.6 Ammonium acetate solution, 10 mmol/l. 4 Apparatus 441 High performance liquid chromatography ~ tandem mass spectrometry (HPLC-MS/MS), 42 Uttrasontegenerator, wit afequoney rom 35 lew 45 kl a 43. Evaporator device, wth waterbath at 40°C & @ A Intpstwwvn.doe88,comp-£048838856125.Ntml 8820.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hw Ame 2a ~ Q 180 17881-2:2016(E) 4A Glass vial, 40 ml with tight closure. 45° Flask, 100 ni. 46 Filtration membrane, 0,45 ym. 4.7 Balance, an accuracy of0,1 mg. 5 Procedure 5.1 Preparation of standard solutions 5.11 Stock standard solution Prepare 1 000 ug/ml stock standard solutions of the acetonitrile (3.5). ndividual flame retardant (8.1 to 3.3) In 54.2 Working solution Prepare an admixture working solution of three flame retardants in acetonitrile and dilute it toa series ‘of sultable concentrations depending on test needs, Select at least five appropriate dilutions of the calibration sets to create calibration curve and perform HPLC-MS/MS analysis. 5.2 Preparation of test specimen Propare a representative test specimen ofthe sample. Cutitinto small pieces and weigh (1,00 + 0,01) g ‘of the pieces with a balance (3,7). 5.3 Ultrasonic wave extraction Putthe pieces into a vial with tight closure (4:4) and add 20 ml of acetone. Place the vial in an ultrasonic ‘generator (4.2) at 40 °C for 40 min Filer and transfer the extract into 100 ml flask (4.5). Add 20 ml of Acetone to the residue and place the vial in the ultrasonic generator to extract the residue at 40 °C for 20 min. Filter and merge the extract into the flask (4.5). Evaporate the extract to near dryness by evaporator device (&.3). Add 2 ml of acetonttrle to dissolve the residue and then filter by filtration membrane (4.6). The filerate is ready for determination of flame retardants. 5.4 Flame retardants determination Determinate the flame retardants in solution (5.a) by HPLC-MS/MS (4.1). The test parameters by HPLC-MS/MS are given in Annex A as an example, Run a blank to control contamination. ‘When the flame retardants level is very low, itis necessary to increase the mass ofthe pieces in order to reach atleast three times the detection int. ‘When the flame retardant level is beyond the linear detector response range of the equipment, its necessary to dilute the specimen liquid properly. 2 (0150 2016- rs eer a Intpstwwvn.doe88,comp-£048838856125.Ntml one20.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hw Ame 2a ~ 180 17881-2:2016(E) 6 Calculation Quantity the concentration of each flame retardant by using the ealibration curve. The content of each flame retardant is expressed by the mass ratio of flame retardant to test specimen, in ug/, Calculate the result by using Formula (1) x, = GS @ where isthe content ofthe flame retardant, in the textile specimen, in 13/8 Gis theconcentration ofthe flame retardant, jin the specimen solution, i g/ml Cs the concentration ofthe flame retardant in the blank solution, in a/ml; V- Isthe final volume ofthe specimen solution, in mi im Is the mass of the test specimen, in g 7 Test report ‘The test report shall include the following information: 8) areference to this part of I80 17881, ie. 180 17881-2:2016; 1) all details necessary for identification ofthe sample tested; ©) the content ofeach flame retardant; any deviation from the procedure specified. & Se (© 190 2016 A rights reserved Boa a REBAR, RAMS CE Fines UC, GSE, RAMEN, LNT, Ren! -ntpswwn.doe88,comp-£048838856125.Ntml s0n820.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hw Ame 2a ~ Q BS EN ISO 17881-2:2016 10 17881-2:2016(E) Annex A (informative) ‘Test parameters by HPLC-MS/MS A. Instrument parameters ‘As 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) Eluent 10 mmol/l ammonium acetate saution; by Eluent 2: Acetonitrile; Chromatographic column: Pursuit XRs C18, 100 mm x 2,0 mm,5 ym; 4) Column temperatures 30°C; ©) Flow rate: 0,2.mi/min; 1) Injection volume: Sou 8) Gradient Time (min) Eluent 2%) ° 10 3 0 10 80 2 9 7 95 171 10 28 10 1h) Detection mode: Quadrupole tandem mass spectrometers; ‘Multiple Reaction Monitoring (MRM); i) nizing mode: Esl electrospray ionizing method and positive-ion detection; 1) Impressed voltage: 5500 vs ig) Temperature of prays 400°C; 1 Spray gas Nitrogen. A.2 Typical transitions and detection ‘Typical transitions and detection limit for flame retardants are shown in Table A. a Se a ‘ (0150 2016- Aight eserves Aa Intpstwwvn.doe88,comp-£048838856125.Ntml 11820.08.23, 14:18 < 16> QQ (hem A we ~ BS ENISO 17881-22016 HS ome 180 17881- ‘Table Al — Typical transitions and detection limit :2016(E) Frecursorion | Production | Detection limit No, Flame retardant (yy) orn (wee) 1 frvis (2.3. 1) ph RIS e986 wn 1 ris (2.3-dibromopropy!) phosphate (TRIS) a 130 2. | ris (airing) phosphineoxide (TEPA) 40 aa 1 23. | vis (z-chloroethy) phosphate (CEP) amp bt) 1 i (2chloroethyl) phosphate (TCEP) a [guaneaive ranston & Se (© 190 2016 A rights reserved @ os a Intpstwwvn.doe88,comp-£048838856125.Ntml 128820.06.23, 18:18, BS ENISO 17881-22016 HS < 16> QQ (hem Awme~ 2a ~ Q 8 180 17881-2:2016(E) Annex B (informative) Round Robin test ‘The Round Robin test was carried out by five textile laboratories in China {A total of nine samples were prepared, three from cotton woven fabrics (ho. 1 to 3), three from polyester woven fabrics (no. 4 to 6) and three from 50 cotton/30 polyester woven fabris (no. 7 to 9} ‘each containing three flame retardants, ie. TRIS, TCEP, and TEPA. The three samples from each fabric ‘wereat three concentration levels of 10 mg/kg, 200 mg/kg, and 500 mg/kg, Three test specimens from ‘each sample were tested in each laboratory. ‘The results ofthe Round Robin test are shown in Table B.. ‘Table B.1 — Results of the Round Robin test same Jpaytance Eta] Mean [Recovery| Sept Reproducbi ro. engyngy | 8/8) | (20) | Setar) | CHE) | SeComerha | CV %) TRIS 10 | 858 | as90 | oss | 40a | oma | 70 1 freer 1 | 096 | sav | ose | sz | 97 | 1005 irePa 10 |_753_| 7527 | 027 | asa | 154 | 2040 iris 200 | 189.56 | 9478 | 1302 | 607 | 2098 | 14.07 2 [reer 200 | 19492 | 746 | ose [a0 | tase | 96 [Tera 200 | 20604 | 10302 | 1573 | 764 | os | 720 Irais 500 | 44373 | oars | ioe | 24s | size | 705 [reap 500 | 45477 | ones | 682 | 173 | 3230 | 710 rea soo | s2a.33 | t0se7 | sz0a_| 7o1_| 4200 | 795 frais 10 | oa | once | 049 | 579 | 100 | i107 4 [reer 10 | 795 | 7940 | o71 | ano | 176 | 2213 IrePA 10 | zoe | 7640 | 027 | ssa | ues | 2305 frais 200 | 17651 | a26 | 745 | 422 | 1553 | a0 s [reer 200 | 19870 | 943s | ata | 433 | ana7_| ona rar 200 | 20453 | 10227 | 1313 [42 | rar | 622 rs 500 | 43735 | ore7_| 1509 | sso | 2n0e | oso 6 [reer 500 | 45661 | 9132 | 1268 | 278 | 2077 | 455 IrePa 500 | 47522 | 9504 | 278 | 521 | mse | 3.069 freis 10 | soa | so36 | 028 | as | 172 | a1as 7 [reer 10 | ese | 524 | o4o | ara | os2 | 1076 freea 10 | 736 | 7360 | 037 | sos | 286 | 3000 frais 200 | aeass | ove | 571 | ai | 954 | 520 8 [reap 200 | 20095 | 10046 | 705 | 3s1_| 1975 | 98s rare 200 | 1952 | 92 | 7as__| aor | 19.20 | 1085 NOTE The results of EPA ar rom hee laboratories a 6 (0150 2016- rs eer a REBADES, RAPRASCE SURF, SSE, RANA, RENT, ReeCMe! eines -ntpswwn.doe88,comp-£048838856125.Ntml 138820.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hem Awme~ 2a ~ Table B.1 (continued) BS EN 150 17881-2:2016 1S0 17881-2:2016(E) sare Jesynnce] REGS] neon [over | — Reve Reproduetblity CS ongiigy [Creed] 0) | Seema/tay | vr (86) | Setonaree) | cv) irae soo | 7596 | 9519 | taro | zee | seas | ae 9 freer soo | 47692 | 9538 | 1560 | 327 | s200_| 1090 ‘Tera soo | so7aa | tras | 6oe | 728 | 2105 | ans & Se a (0150 2016- Agha 7 Aa Intpstwwvn.doe88,comp-£048838856125.Ntml 148820.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hw Ame 2a ~ Q his page deiverately Be blank Aa Intpstwwvn.doe88,comp-£048838856125.Ntml 191820.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hw Ame 2a ~ Q nispage deinerately Be blank Aa RBA, DH MESSY SUAS, ERE, SHIR, LET, BemIORE! Fer -ntpswwn.doe88,comp-£048838856125.Ntml 18820.08.23, 14:18 BS ENISO 17881-22016. sHES < 6 > @Q (Dawe Ate -~ 2 mt ~ e Vo orn THOUS SSN OCA RUTIDB CoP British Standards Institution (BSI) 1 ing British St andards and other standardizatio About us Revisions See sn saeco nine vain Bee ag iran Lee ee romertinweieematamine Seaaacnemiaaee naneretececry —cobpi emer i Infomation on standards an Reeneetpenaetieeds inet carat” Pea a armas ee ae eee ae Ree SRST, iment eer men Sees eeieeers eae ee eee ee a Somer areata ne ees oe Paying standards famdenn eget See eer eee Uta comma: ipereina vel nscsoemse ee ane Cocmciacincumcicrmeanasie Sastage See eee sem wee oe. in bc a ao A Src Soree temo Se an Rec eealciieiicieenee i fiemansaty Seesmic Hae, betel celery eae alas cuumerte puna uate ngs cyanea eng Fusbonsiargevieersontetiactog aces ow Em arson am capers ais gene Sete dat ible eset le sea pemme neat gan paeenicce eee ees ae Eola rp rege eer aoe, scp Mangus . bsi : Sl. a A RAR, Sw EEL connie BURY, ORL, UR, SHPI, RETHORE! po dos. com 804860896125 rl m820.08.23, 14:18 BS ENISO 17881-22016 HS < 16> QQ (hw Ame 2a ~ SURO, CUTER Bicones eva ERE? FEXORE Feentonnwczts (ORT SAORI T ee: oven 50 oIveN so ASN SOGHEIE- SEN SOOHSDE- SEN BO ODIST- Vreer-22016-09- 178ET2E OED 3.2016 pes zor name ae Binge RM Bape EA) xrawe muna an same a2 pus 1 mae) wren meee Intpstwwvn.doe88,comp-£048838856125.Ntml 35 EN 150 058 $2016 Omer & Se a A eee serene 188