1、BS EN 15777:2009ICS 59.080.01NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDTextiles Test methodfor phthalatesLicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 15/01/2010 02:15, Uncontrolled Copy, (c) BSIThis British Standardwas published underthe authorit
2、y of theStandards Policy andStrategy Committee on 30November 2009. BSI 2009ISBN 978 0 580 61527 6Amendments/corrigenda issued since publicationDate CommentsBS EN 15777:2009National forewordThis British Standard is the UK implementation of EN 15777:2009.The UK participation in its preparation was ent
3、rusted to TechnicalCommittee TCI/80, Chemical testing of textiles.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application
4、.Compliance with a British Standard cannot confer immunityfrom legal obligations.Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 15/01/2010 02:15, Uncontrolled Copy, (c) BSIBS EN 15777:2009EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15777August 2009ICS 59.080.01English VersionTextiles -
5、 Test method for phthalatesTextiles - Mthodes dessai des phtalates Textilien - Prfverfahren fr PhthalateThis European Standard was approved by CEN on 24 July 2009.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard
6、 the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, Ger
7、man). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Rep
8、ublic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NO
9、RMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: Avenue Marnix 17, B-1000 Brussels 2009 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15777:2009: ELicensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 15/01/2010 02:15,
10、Uncontrolled Copy, (c) BSIBS EN 15777:2009EN 15777:2009 (E) 2 Contents Page Foreword 3Introduction .41 Scope 52 Terms and definitions .53 Preparation of the test specimens .54 Apparatus and reagents 54.1 Apparatus .54.2 Reagents (analytical grade) 65 Test procedure .65.1 Principle 65.2 Reagent (stan
11、dard solutions) .65.3 Extraction of phthalates 75.4 Calculation of results 76 Test report 8Annex A (normative) Calculations .9A.1 Overall treated 9A.2 Locally treated . 10Annex B (informative) Suitable Gas Chromatography - Mass Spectrometry (GC-MS) apparatus, method and precision data for determinat
12、ion of phthalate plasticizers 3 11Bibliography . 13Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 15/01/2010 02:15, Uncontrolled Copy, (c) BSIBS EN 15777:2009EN 15777:2009 (E) 3 Foreword This document (EN 15777:2009) has been prepared by Technical Committee CEN/TC 248 “Textile and textile pr
13、oducts”, 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 by February 2010, and conflicting national standards shall be withdrawn at the latest by February 201
14、0. 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 organizat
15、ions of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Licensed Copy: Wang Bin,
16、 ISO/EXCHANGE CHINA STANDARDS, 15/01/2010 02:15, Uncontrolled Copy, (c) BSIBS EN 15777:2009EN 15777:2009 (E) 4 Introduction This European Standard covers a test method for determination of phthalates in textile articles. Phthalates are commonly used as plasticizers in polymers. Toxicological concern
17、 has arisen due to their potential effect as endocrine disruptors and some of the listed phthalates are toxic in reproduction. The level of media publicity will ensure that their use will continue to be of concern to consumers. Phthalates are an issue for textile manufacturers and retailers due to t
18、heir use within motifs, coated fabrics, plastisol prints, buttons, etc. There are textile articles that have to comply with the Directive 2005/84/EC 1 and also articles that fall outside the scope of this legislation, that could be covered by the General Products Safety Directive (2001/95/EC) 2. WAR
19、NING Persons using this European Standard should be familiar with normal laboratory practice. This European Standard does not claim to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to
20、 ensure compliance with any national regulatory conditions. This European Standard calls for the use substances and/or procedures that may be injurious to health if appropriate precautions are not observed. It refers only to technical suitability and does not absolve the user from legal obligations
21、relating to health and safety at any stage. Phthalates are controversial because high doses of many phthalates have shown hormonal activity in rodent studies. Studies on rodents involving large amounts of phthalates have shown damage to the liver, the kidneys, the lungs, and the developing testes. I
22、MPORTANT It is absolutely essential that tests conducted according to this European Standard be carried out by suitably trained staff. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 15/01/2010 02:15, Uncontrolled Copy, (c) BSIBS EN 15777:2009EN 15777:2009 (E) 5 1 Scope This standard specifie
23、s a test method for taking representative specimens, extraction of phthalates from the material and determination of phthalates by gas chromatography mass spectrometry. This standard applies to textiles articles, where there is a possibility of the presence of some phthalates. 2 Terms and definition
24、s For the purposes of this European Standard, the following terms and definitions apply. 2.1 blank application of the method without test specimen 2.2 plasticized or softened materials plastic material (coating, pigment print binder, etc) that is treated with chemicals (for this specific standard th
25、ey are phthalates) to make it more flexible 2.3 overall treated textiles textiles with a continuous finish, coating or print 2.4 locally treated textiles textile with a discontinuous finish, coating or print 2.5 representative specimen specimen obtained by mixing pieces of all the different treated
26、parts and colours 3 Preparation of the test specimens Remove the untreated mass of the specimen if possible (see Annex A). If the untreated mass cannot be removed, see 5.4. Use a scalpel or other appropriate cutting tool to cut two representative specimens into small pieces. 4 Apparatus and reagents
27、 4.1 Apparatus 4.1.1 Balance (resolution of 1 mg). 4.1.2 150 ml flask. 4.1.3 Soxhlet extractor with siphon cup of approximately 20 ml. 4.1.4 Soxhlet cellulose thimble, approximately 15 mm in diameter and 50 mm height. 4.1.5 Water-cooled condenser. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARD
28、S, 15/01/2010 02:15, Uncontrolled Copy, (c) BSIBS EN 15777:2009EN 15777:2009 (E) 6 4.1.6 Spark proof heating mantle/water bath. 4.1.7 Steam bath or rotary evaporator. 4.1.8 Calibrated volumetric flasks of suitable volume. NOTE Avoid direct contact between the samples and glassware and/or equipment t
29、o be used to minimize cross-contamination. Glassware, after washing, should have an extra rinse with 0,1 N nitric acid and finally with acetone, acetone/methanol and/or cyclohexane. Dry at 110 C (1 h). Beware, the vapour of the organic solvents are highly flammable, especially at high temperature! A
30、llow glassware to cool down before use. 4.1.9 Gas chromatography with mass selective detector (GC-MS). 4.2 Reagents (analytical grade) 4.2.1 n-Hexane, CAS No. 110-54-3. 4.2.2 Di-isononyl phthalate (DINP), CAS No. 28553-12-0 or 68515-48-0. 4.2.3 Di-(2-ethylhexyl) phthalate (DEHP), CAS No. 117-81-7. 4
31、.2.4 Di-n-octyl phthalate (DNOP), CAS No. 117-84-0. 4.2.5 Di-iso-decyl phthalate (DIDP), CAS No. 26761-40-0 or 68515-49-1. 4.2.6 Butyl benzyl phthalate (BBP), CAS No. 85-68-7. 4.2.7 Di-butyl phthalate (DBP), CAS No.84-74-2. 4.2.8 Dicyclohexyl phthalate (DCHP), CAS no.84-61-7 Internal Standard. 5 Tes
32、t procedure 5.1 Principle The aim of the method is to extract phthalates in textiles and related accessories. This method uses Soxhlet extraction apparatus with n-hexane as solvent. However, any apparatus giving equivalent extraction as with Soxhlet can be used. The total n-hexane extractable phthal
33、ate plasticizer content is calculated by weight with Gas Chromatography-Mass-Spectrometry (GC-MS) detection to identify and quantify individual phthalates. 5.2 Reagent (standard solutions) 5.2.1 Preparation of the internal standard solution. Prepare a 500 g/ml stock solution of the internal standard
34、 in n-hexane. 5.2.2 Standard solution. Prepare a series of individual stock standard solutions of the individual phthalate in n-hexane as shown in Table 1. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 15/01/2010 02:15, Uncontrolled Copy, (c) BSIBS EN 15777:2009EN 15777:2009 (E) 7 Table 1 S
35、tock solutions Phthalate DIDP DINP DBP BBP DNOP DEHP Concentration, g/ml 1000 1000 200 200 200 200 From the stock standard solutions prepare appropriate phthalate calibration solutions in n-hexane. Use at least five appropriate dilutions of the calibration sets to create calibration graphs and add t
36、o each an appropriate amount of internal standard and perform GC-MS analysis. NOTE DIDP and DINP overlap in the chromatogram, choose target ions indicated in Annex B. 5.3 Extraction of phthalates Prepare the appropriate amount of internal standard solution. Weigh accurately (2,0 0,1) g of the pieces
37、 of a representative specimen into a Soxhlet thimble and add a filter paper disc to the top of the thimble. Extract every sample in duplicate and run a blank to control contamination. Add approximately 50 ml of n-hexane into the flask. Reflux gently for 4 h. Allow sufficient time for the n-hexane to
38、 cool. Transfer the extract to a 100 ml volumetric flask. Rinse the flask with 2 aliquots of 20 ml n-hexane. Make up to the mark. Transfer a known volume into a suitable GC sampling vial and add appropriate volume of internal standard solution and perform GC-MS analysis. Prepare if necessary further
39、 diluted solutions using the original solution and repeat the analysis after added the appropriate volume of internal standard solution. NOTE In some cases where the corrected mass of the specimen is very low, it will be necessary to increase the weight and/or concentrate the extract in order to rea
40、ch at least 3 times the detection limit. 5.4 Calculation of results From the calibration graph determine the response of each phthalate, corrected for the internal standard peak area, and interpolate the concentration of the phthalate in g/ml correcting for any dilutions. Subtract the blank concentr
41、ation from the specimen concentration. 10000ma - b=VP (1) where P is the percentage of the individual phthalate; V is the volume of the volumetric flask (ml); m is the corrected mass of specimen (g); a is the concentration of the individual phthalate of blank solution (g/ml); b is the concentration
42、of the individual phthalate the specimen solution corrected for any dilutions (g/ml). If the corrected mass of test specimen cannot be obtained (see Annex A), give a remark in the test report. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 15/01/2010 02:15, Uncontrolled Copy, (c) BSIBS EN 15
43、777:2009EN 15777:2009 (E) 8 An example of the calculation is given in Annex A. Overall treated material is illustrated in Figure A.1 and locally treated material in Figure A.2. 6 Test report The test report shall include the following information: a) reference to this standard; b) all details necess
44、ary for complete identification of the sample tested; c) description of the apparatus if Soxhlet is not used; d) preparation of the specimens and correction of the mass due to the untreated textile components; e) percent by mass of each listed phthalate in the plasticized material or textile product
45、; f) any deviation by agreement or otherwise from the procedure specified. Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 15/01/2010 02:15, Uncontrolled Copy, (c) BSIBS EN 15777:2009EN 15777:2009 (E) 9 Annex A (normative) Calculations A.1 Overall treated In the case of overall treated specim
46、ens, see Figure A.1: 12Key 1 Plastic Component (Coating) 2 Fabric Figure A.1 Overall treated materials 1m = total mass of overall treated specimen (g); 2m = mass of textile component (g); m = mass of coating (g) NOTE Mass of coating is the corrected mass of the specimen as described in the formula i
47、n 5.4. From a test specimen, where (1m ) is measured (g), the plastic component (coating) is removed by a mechanical, thermal or chemical procedure (or combination of these). The plastic component ( m ) shall be determined by comparison with the textile component (2m ). The part of the coating can b
48、e defined according to the following formula: 21mmm = (A.1) Licensed Copy: Wang Bin, ISO/EXCHANGE CHINA STANDARDS, 15/01/2010 02:15, Uncontrolled Copy, (c) BSIBS EN 15777:2009EN 15777:2009 (E) 10 A.2 Locally treated In the case of locally treated specimens, see Figure A.2. 21Key 1 Plastic Component
49、(Coating) 2 Fabric Figure A.2 Locally treated specimen 1m = mass per unit area of treated area of specimen (gm-2); 2m = mass per unit area of textile material (gm-2); m = mass of the plastic component (coating) (g); NOTE Mass of the plastic component is the corrected mass of the specimen as described in the formula in 5.4. S = surface area of the treated area of the specimen (m2); Firstly, determine the mass per unit area from an untreated part (only textile material is involved)
