1、October 2014 Translation by DIN-Sprachendienst.English price group 14No 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).IC
2、S 59.080.01!%;IJ“2243839www.din.deDDIN EN ISO 14389Textiles Determination of the phthalate content Tetrahydrofuran method (ISO 14389:2014);English version EN ISO 14389:2014,English translation of DIN EN ISO 14389:2014-10Textilien Bestimmung des Phthalatanteils Tetrahydrofuran-Verfahren (ISO 14389:20
3、14);Englische Fassung EN ISO 14389:2014,Englische bersetzung von DIN EN ISO 14389:2014-10Textiles Dtermination de la teneur en phtalates Mthode au ttrahydrofurane (ISO 14389:2014);Version anglaise EN ISO 14389:2014,Traduction anglaise de DIN EN ISO 14389:2014-10SupersedesDIN EN 15777:2009-12www.beut
4、h.deDocument comprises 28 pagesIn case of doubt, the German-language original shall be considered authoritative.09.14 DIN EN ISO 14389:2014-10 2 A comma is used as the decimal marker. National foreword This document (EN ISO 14389:2014) has been prepared by Technical Committee ISO/TC 38 “Textiles” in
5、 collaboration with Technical Committee CEN/TC 248 “Textiles and textile products” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was the DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-05-12 AA Tex
6、tilchemische Prfverfahren und Fasertrennung. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 1833-1 DIN EN ISO 1833-1 ISO 5725-2 DIN ISO 5725-2 ISO 5725-5 DIN ISO 5725-5 Amendments This standard differs from DIN EN 15777:2009-12 as foll
7、ows: a) the text of ISO 14389:2014 has been adopted; b) tetrahydrofuran is now used as a reagent; c) the method for the determination of the phthalate content has been changed. Previous editions DIN EN 15777: 2009-12 National Annex NA (informative) Bibliography DIN EN ISO 1833-1, Textiles Quantitati
8、ve chemical analysis Part 1: General principles of testing DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN ISO 5725-5, Accuracy (trueness and prec
9、ision) of measurement methods and results Part 5: Alternative methods for the determination of the precision of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14389 June 2014 ICS 59.060.01 Supersedes EN 15777:2009English Version Textiles - Determination of the
10、 phthalate content - Tetrahydrofuran method (ISO 14389:2014) Textiles - Dtermination de la teneur en phtalates - Mthode au ttrahydrofurane (ISO 14389:2014) Textilien - Bestimmung des Phthalatanteils - Tetrahydrofuran-Verfahren (ISO 14389:2014) This European Standard was approved by CEN on 20 June 20
11、14. 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 alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained
12、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 made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CEN
13、ELEC 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, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Ita
14、ly, Latvia, 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: Ave
15、nue 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 EContents PageForeword 3Introduction 41 Scope . 52 Terms and definitions . 53 Principle 54 Reagents 55 Apparatus . 66 Procedure . 76
16、.1 Preparation of standard solutions . 76.2 Ultrasonic extraction and determination of phthalates 87 Calculation of the results . 97.1 Calculation based on the corrected mass (by default) 97.2 Calculation based on the total mass (when relevant) 108 Test report 11Annex A (normative) Calculations . 12
17、Annex B (informative) Example of test parameters by GC-MS 14Annex C (informative) Determination of PVC mass fraction by chemical method 16Annex D (informative) Statistical data.19Bibliography .26DIN EN ISO 14389:2014-10EN ISO 14389:2014 (E)2 DIN EN ISO 14389:2014-10 EN ISO 14389:2014 (E)3Foreword Th
18、is 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 status of a national standard, either
19、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 subject of patent rights. CEN and/o
20、r 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 this European Standard: Austria, Be
21、lgium, 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, Swit
22、zerland, 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. IntroductionThis International Standard covers a test method for the determination of some phthalates in textile articles.Phthalates are commo
23、nly used as 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. Stud
24、ies on rodents 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 b
25、een restricted in some regulations (e.g. in the European Union).DIN EN ISO 14389:2014-10EN ISO 14389:2014 (E)4 WARNING This International Standard calls for the use of substances and/or procedures that might be injurious to health if adequate precautions are not taken. It refers only to technical su
26、itability 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 experienced operators.1 ScopeThis Internation
27、al 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 there is a risk of the presence of some phthalates.2 Terms and definitionsFor the pur
28、poses 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 International Standard, the chemicals are phthalates.EXAMPLE Examples of plastic material: c
29、oating, 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 specimenspecimen obtained by mixing pieces of all the different treated parts and colours3 Pr
30、incipleThe 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 precipitation of the dissolved polymer using the appropriate solvent (acetonitrile, n-hexane
31、, 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 standard (IS).4 ReagentsUnless otherwise specified, use only reagents of recognized analyt
32、ical grade.DIN EN ISO 14389:2014-10 EN ISO 14389:2014 (E)5 4.1 Tetrahydrofuran (THF), CAS number: 109-99-9.4.2 Solvents used for the precipitation. Examples 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, inter
33、nal 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-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 (
34、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 (DPP), 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-
35、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, 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
36、 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.DIN EN ISO 14389:2014-10EN ISO 14389:2014 (E)6 6 ProcedureWARNING The vapour of the organic solvents is highly flammable, especially at high tempe
37、rature. Allow glassware to cool down before use.Avoid direct contact between the samples and glassware and/or equipment used in order to 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
38、completely dried before use. To avoid contamination, do not use any plastic container (e.g. for water).6.1 Preparation of standard solutions6.1.1 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
39、ultrasonic extraction (see 6.2).6.1.2 Preparation of stock standard solutionsPrepare a series of individual stock standard solutions of the 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 a
40、nd fill the volumetric flask up to the mark with the solvent used for the precipitation and mix thoroughly to dissolve completely the substance.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
41、 may be made in a mixed stock. This saves time and effort when preparing calibration solutions. DINP, DIDP and DIHP have overlapping peaks. 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 th
42、e other phthalates because of their multi-peak nature. Hence, the higher limit of detection in Annex B.6.1.3 Preparation of the calibration solutionsFrom the stock standard solutions, prepare at least five appropriate phthalate calibration solutions (example of concentrations at 1 mg/l, 3 mg/l, 15 m
43、g/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 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 tetrahyd
44、rofuran to 66 parts of the other solvent), as shown in Table 2. Each calibration solution should have a final internal standard concentration 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 p
45、roper retention times and the absence of contamination and built up the calibration curve.DIN EN ISO 14389:2014-10 EN ISO 14389:2014 (E)7 Table 2 Examples of calibration solutionsConcentration InstructionsBlank In a 50 ml volumetric flask, add 0,25 ml of internal standard (DCHP) stock solution; then
46、, fill up to the mark with 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)1 mg/l Add 0,1 ml of each stock standard solution in 100 ml volumetric flask plus 0,5 ml of the internal st
47、andard (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-drofuran to 66 parts of the solvent used for the precipitation.15 mg/l Add 0
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