1、BSI Standards PublicationBS EN ISO 14389:2014Textiles Determination of the phthalate content Tetrahydrofuran methodIncorporating corrigendum July 2014BS EN ISO 14389:2014National forewordThis British Standard is the UK implementation of EN ISO 14389:2014. It supersedes BS EN 15777:2009 which is with
2、drawn.The UK participation in its preparation was entrusted to Technical Committee TCI/80, Chemical testing of textiles.A list 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 con
3、tract. Users are responsible for its correct application. The British Standards Institution 2014. Published by BSI Standards Limited 2014ISBN 978 0 580 87275 4ICS 59.060.01Compliance with a British Standard cannot confer immunity from legal obligations.This British Standard was published under the a
4、uthority of the Standards Policy and Strategy Committee on 31 July 2014.Amendments/corrigenda issued since publicationDate Text affected31 July 2014 Implementation of CEN Correction Notice 18 June 2014: Supersession information updatedBRITISH STANDARDEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM
5、 EN ISO 14389 June 2014 ICS 59.060.01 Supersedes EN 15777:2009English Version Textiles - Determination of the phthalate content - Tetrahydrofuran method (ISO 14389:2014) Textiles - Dtermination de la teneur en phtalates - Mthode au ttrahydrofurane (ISO 14389:2014) Textilien - Bestimmung des Phthalat
6、anteils - Tetrahydrofuran-Verfahren (ISO 14389:2014) This European Standard was approved by CEN on 20 June 2014. CEN members 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 al
7、teration. 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 official versions (English, French, German). A version in any other language m
8、ade 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 of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Est
9、onia, 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. EUROPEAN COMMITTEE FOR STA
10、NDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 14389:2014 EBS EN ISO 14389:2014EN
11、 ISO 14389:2014 (E) 3 Foreword This document (EN ISO 14389:2014) 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 statu
12、s of a national standard, either by publication of an identical text or by endorsement, at the latest by December 2014, and conflicting national standards shall be withdrawn at the latest by December 2014. Attention is drawn to the possibility that some of the elements of this document may be the su
13、bject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 15777:2009. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement th
14、is 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, Slovak
15、ia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 14389:2014 has been approved by CEN as EN ISO 14389:2014 without any modification. BS EN ISO 14389:2014ISO 14389:2014(E) ISO 2014 All rights reserved iiiContents PageForeword ivIntroduction v1
16、 Scope . 12 Terms and definitions . 13 Principle 14 Reagents 15 Apparatus . 26 Procedure. 36.1 Preparation of standard solutions . 36.2 Ultrasonic extraction and determination of phthalates 47 Calculation of the results . 57.1 Calculation based on the corrected mass (by default) 57.2 Calculation bas
17、ed on the total mass (when relevant) . 68 Test report . 7Annex A (normative) Calculations 8Annex B (informative) Example of test parameters by GC-MS 10Annex C (informative) Determination of PVC mass fraction by chemical method 12Annex D (informative) Statistical data.15Bibliography .22BS EN ISO 1438
18、9:2014ISO 14389:2014(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
19、 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 ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commissio
20、n (IEC) 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
21、 be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2. www.iso.org/directivesAttention 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 identifying
22、 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. www.iso.org/patentsAny trade name used in this document is information given for the convenience of users
23、 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 - Supplementary
24、 informationThe committee responsible for this document is ISO/TC 38, Textiles.iv ISO 2014 All rights reservedBS EN ISO 14389:2014ISO 14389:2014(E)IntroductionThis International Standard covers a test method for the determination of some phthalates in textile articles.Phthalates are commonly used as
25、 plasticizers in polymers. Phthalates are an issue for textile manufacturers and retailers due to their use within motifs, coated fabrics, plastisol prints, buttons, etc.Phthalates are controversial because high doses of many phthalates have shown hormonal activity in rodent studies. Studies on rode
26、nts involving large amounts of phthalates have shown damage to the liver, the kidneys, the lungs, and the developing testes.Due to their potential effect as endocrine disruptors, some of the listed phthalates are toxic in reproduction. The listed phthalates are based on those which have been restric
27、ted in some regulations (e.g. in the European Union). ISO 2014 All rights reserved vBS EN ISO 14389:2014BS EN ISO 14389:2014Textiles Determination of the phthalate content Tetrahydrofuran methodWARNING This International Standard calls for the use of substances and/or procedures that might be injuri
28、ous to health if adequate 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 ent
29、rusted to appropriately qualified and experienced operators.1 ScopeThis International Standard specifies a method of determining phthalates in textiles with gas chromatographymass spectrometry (GC-MS) with mass selective detector.This International Standard is applicable to textile products where th
30、ere is a risk of the presence of some phthalates.2 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.2.1plasticized or softened materialplastic material that is treated with chemicals to make it more flexibleNote 1 to entry: For this specific Internati
31、onal Standard, the chemicals are phthalates.EXAMPLE Examples of plastic material: coating, pigment print binder, etc.2.2overall treated textiletextile with a continuous finish, coating or print2.3locally treated textiletextile with a discontinuous finish, coating or print2.4representative specimensp
32、ecimen obtained by mixing pieces of all the different treated parts and colours3 PrincipleThe phthalates are extracted from textile specimen by ultrasonic generator with tetrahydrofuran. As the plastic polymer is partially or completed dissolved, the phthalate extraction is followed by the precipita
33、tion of the dissolved polymer using the appropriate solvent (acetonitrile, n-hexane, etc.). After centrifugation and dilution of the extract to volume, gas chromatographymass spectrometry (GC-MS) is used to identify individual phthalates in the specimen and quantify them by using an internal standar
34、d (IS).4 ReagentsUnless otherwise specified, use only reagents of recognized analytical grade.INTERNATIONAL STANDARD ISO 14389:2014(E) ISO 2014 All rights reserved 1BS EN ISO 14389:2014ISO 14389:2014(E)4.1 Tetrahydrofuran (THF), CAS number: 109-99-9.4.2 Solvents used for the precipitation. Examples
35、are:4.2.1 Acetonitrile, CAS number: 75-05-8.4.2.2 n-Hexane, CAS number: 110-54-3.4.3 Di-cyclohexyl phthalate (DCHP), CAS number: 84-61-7, internal standard (IS).4.4 Di-isononyl phthalate (DINP), CAS number 28553-12-0 or 68515-48-0.4.5 Di-(2-ethylhexyl) phthalate (DEHP), CAS number 117-81-7.4.6 Di-n-
36、octyl phthalate (DNOP), CAS number 117-84-0.4.7 Di-iso-decyl phthalate (DIDP), CAS number 26761-40-0 or 68515-49-1.4.8 Butyl benzyl phthalate (BBP), CAS number 85-68-7.4.9 Di-butyl phthalate (DBP), CAS number 84-74-2.4.10 Di-iso-butyl phthalate (DIBP), CAS number 84-69-5.4.11 Di-pentyl phthalate (DP
37、P), CAS number: 131-18-0.4.12 Di-iso-heptyl phthalate (DIHP), CAS number: 71888-89-6.4.13 Di-methoxyethyl phthalate (DMEP), CAS number: 117-82-8.5 Apparatus5.1 Gas chromatograph-mass spectrometer (GC-MS), with mass selective detector (MSD).5.2 Vial, of capacity 40 ml.5.3 Thermostatic ultrasonic bath
38、, with a frequency of (40 5) kHz.5.4 Glass flasks with glass stoppers, of capacity 100 ml.5.5 Calibrated volumetric flasks, of capacities 50 ml and 100 ml.5.6 Volumetric graduated pipette, of capacities 10 ml and 20 ml.5.7 Balance, with a resolution of 0,1 mg.5.8 Water bath.5.9 Rotary evaporator.2 I
39、SO 2014 All rights reservedBS EN ISO 14389:2014ISO 14389:2014(E)6 ProcedureWARNING The vapour of the organic solvents is highly flammable, especially at high temperature. Allow glassware to cool down before use.Avoid direct contact between the samples and glassware and/or equipment used in order to
40、minimize cross-contamination. Glassware, after washing, should be given an extra rinse with 0,1 N nitric acid, water and finally with acetone. Glassware should be completely dried before use. To avoid contamination, do not use any plastic container (e.g. for water).6.1 Preparation of standard soluti
41、ons6.1.1 Internal standard solutionPrepare a 1 000 mg/l stock standard solution of the internal standard in the solvent used for the precipitation (4.2) after the ultrasonic extraction (see 6.2).6.1.2 Preparation of stock standard solutionsPrepare a series of individual stock standard solutions of t
42、he individual phthalate ester in the solvent used for the precipitation as shown in Table 1.For example, weigh 50,0 mg of a phthalate in a 50 ml volumetric flask and fill the volumetric flask up to the mark with the solvent used for the precipitation and mix thoroughly to dissolve completely the sub
43、stance.Table 1 Stock standard solutionsPhthalate esterDCHP (IS) DINP DEHP DNOP DIDP BBP DBP DIBP DPP DIHP DMEPConcen- tration, mg/l1 000Most of the stock standards may be made in a mixed stock. This saves time and effort when preparing calibration solutions. DINP, DIDP and DIHP have overlapping peak
44、s. It is recommended to make up these stock standard solutions separately, as their calibration solutions have to be made in higher (5x) concentrations than for the other phthalates because of their multi-peak nature. Hence, the higher limit of detection in Annex B.6.1.3 Preparation of the calibrati
45、on solutionsFrom the stock standard solutions, prepare at least five appropriate phthalate calibration solutions (example of concentrations at 1 mg/l, 3 mg/l, 15 mg/l, 30 mg/l and 90 mg/l as described in the Table 2), each containing an equal amount of the target phthalates (4.4 through 4.13) and an
46、 amount of internal standard (4.3) in a mixture of tetrahydrofuran and the solvent used for the precipitation, mixed by volume at a ratio of 1:2 (33 parts tetrahydrofuran to 66 parts of the other solvent), as shown in Table 2. Each calibration solution should have a final internal standard concentra
47、tion of 5 mg/l. Prepare one calibration blank. Analyse the calibration solutions and calibration blank with the GC-MS. Qualitatively analyse the result to ensure proper retention times and the absence of contamination and built up the calibration curve. ISO 2014 All rights reserved 3BS EN ISO 14389:
48、2014ISO 14389:2014(E)Table 2 Examples of calibration solutionsConcentration InstructionsBlank In a 50 ml volumetric flask, add 0,25 ml of internal standard (DCHP) stock solution; then, fill up to the mark with a mixture of tetrahydrofuran and the solvent used for the precipitation, mixed by volume a
49、t a ratio of 1:2 (33 parts tetrahydrofuran to 66 parts of the other solvent)1 mg/l Add 0,1 ml of each stock standard solution in 100 ml volumetric flask plus 0,5 ml of the internal standard (DCHP) stock solution; then, fill up to the mark with a mixture of 33 parts of tetrahy-drofuran to 66 parts of the solvent used for the precipitation.3 mg/l Add 0,3 ml of each stock standard solution in 100 ml volumetric flask plus 0,5 ml of the internal standard (DCHP) stock solution; then, fill up to the mark with a mixture of 33 parts of tetrahy-dro
