1、September 2016 English price group 11No 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!%$m“2560174www.din.d
2、eDIN EN ISO 18254-1Textiles Method for the detection and determination of alkylphenol ethoxylates (APEO) Part 1: Method using HPLC-MS (ISO 18254-1:2016);English version EN ISO 18254-1:2016,English translation of DIN EN ISO 18254-1:2016-09Textilien Verfahren zum Nachweis und zur Bestimmung von Alkylp
3、henolethoxylaten (APEO) Teil 1: Verfahren unter Verwendung von HPLC-MS (ISO 18254-1:2016);Englische Fassung EN ISO 18254-1:2016,Englische bersetzung von DIN EN ISO 18254-1:2016-09Textiles Mthode de dtection et de dtermination des alkylphnols thoxyls (APEO) Partie 1: Mthode utilisant la CLHP-SM (ISO
4、18254-1:2016);Version anglaise EN ISO 18254-1:2016,Traduction anglaise de DIN EN ISO 18254-1:2016-09www.beuth.deDocument comprises 17 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.08.16 DIN EN ISO 18254-1:2016-09 2 A comma is
5、 used as the decimal marker. National foreword This document (EN ISO 18254-1:2016) has been prepared 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 involv
6、ed in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-05-12 AA Textilchemische Prfverfahren und Fasertrennung. In addition to the legal units of measurement, this standard also uses the unit “psi”. It should, however, be no
7、ted that the Gesetz ber Einheiten im Messwesen (German Law on units in metrology) prohibits the use of this unit for official and commercial purposes in Germany. The indication of this unit solely serves to facilitate the communication with those countries where this unit is used (import-export busi
8、ness). Conversion: 1 psi = 6 894,757 Pa = 0,068 947 57 bar The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 13528 DIN ISO 13528 National Annex NA (informative) Bibliography DIN ISO 13528, Statistical methods for use in proficiency testing b
9、y interlaboratory comparisons EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 18254-1 April 2016 ICS 59.080.01 English Version Textiles - Method for the detection and determination of alkylphenol ethoxylates (APEO) - Part 1: Method using HPLC - MS (ISO 18254-1:2016) Textiles - Mthode de dte
10、ction et de dtermination des alkylphnols thoxyls (APEO) - Partie 1: Mthode utilisant la CLHP-SM (ISO 18254-1:2016) This European Standard was approved by CEN on 2 January 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Eu
11、ropean 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 official versi
12、ons (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 of Austria,
13、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, Sw
14、itzerland, Turkey andUnited 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 for CEN natio
15、nal Members. Ref. No. EN ISO 18254-1:2016 ETextilien - Verfahren zum Nachweis und zur Bestimmungvon Alkylphenolethoxylaten (APEO) - Teil 1: Verfahrenunter Verwendung von HPLC-MS (ISO 18254-1:2016) European foreword .3Introduction 51 Scope . 62 Principle 63 Reagents 64 Apparatus . 74.1 Apparatus and
16、auxiliaries for preparing the sample . 74.2 Chromatographic equipment . 75 Procedure. 75.1 Standard preparation 75.2 Sample preparation 85.3 Analysis 86 Calculation of results . 86.1 Determination of the R value for each congener of APEO . 86.2 Calibration curve . 86.3 Calculation of concentration o
17、f APEO result . 97 Test report . 9Annex A (informative) Examples of chromatographic method LC/MS 10Annex B (informative) Examples of chromatographic method LC/MS/MS . 13Bibliography .15Contents PageDIN EN ISO 18254-1:2016-09 EN ISO 18254-1:2016 (E)2Foreword 4European foreword This document (EN ISO 1
18、8254-1:2016) 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 publication of a
19、n identical text or by endorsement, at the latest by October 2016, and conflicting national standards shall be withdrawn at the latest by October 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 b
20、e 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, Es
21、tonia, 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 notice Th
22、e text of ISO 18254-1:2016 has been approved by CEN as EN ISO 18254-1:2016 without any modification. DIN EN ISO 18254-1:2016-09 EN ISO 18254-1:2016 (E)3 ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The wo
23、rk 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 and non-governm
24、ental, 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 described in th
25、e 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 drawn to the possi
26、bility 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 the ISO list of
27、 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, as well as i
28、nformation about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information.ISO 18254-1 was prepared by the European Committee for Standardization (CEN) in collaboration with ISO Technical Committee ISO/TC 38, Textiles, a
29、nd Technical Committee CEN/TC 248, Textiles and textile products in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).ISO 18254 consists of the following parts under the general title Textiles Method for the detection and determination of alkylphenol ethox
30、ylates (APEO): Part 1: Method using HPLC-MSThe following part is under preparation: Part 2; Method using NPLCDIN EN ISO 18254-1:2016-09 EN ISO 18254-1:2016 (E)4 IntroductionAlkylphenol ethoxylates (APEOs) are high-value products commonly used in industrial and consumer detergents and cleaners, some
31、plastics and many industrial applications. Their “down the drain” uses may result in their presence in wastewater streams and receiving water bodies. Human exposure to APEO can occur through diverse sources such as environmental, food, or skin contact. Considering their toxicity on several animal sp
32、ecies, minimization of exposure to APEO is recognized as important to the preservation of human health.Nonylphenol ethoxylates belong to the non-ionic surfactant category and are of particular concern. The biodegradation of nonylphenol ethoxylate releases the branched nonylphenol, which is difficult
33、 to biodegrade. Nonylphenol is a substance having endocrine disruptive properties that can have serious effects on aquatic and many other organisms. For this reason, the release of nonylphenol ethoxylate into the environment should be avoided.Chemical products containing nonylphenol and/or nonylphen
34、ol ethoxylates in concentrations equal to or greater than 0,1 % are restricted within the EU for specific uses, among others, the processing of leather and textiles, industrial, and institutional cleaning.This restriction is part of the entry 46 of Annex XVII of the REACH regulation EU 1907/2006, wh
35、ich repealed the former Directive 2003/53/EC.The current restriction is due to be widened to apply to textile products that can be washed in water. A limit value of 0,01 % (100 ppm) is expected.DIN EN ISO 18254-1:2016-09 EN ISO 18254-1:2016 (E)5 SAFETY PRECAUTIONS It is the users responsibility to u
36、se safe and proper techniques in handling materials in this test method. Consult manufacturers for specific details such as material safety, data sheets, and other recommendations. Good laboratory practice should be followed. Users should comply with any national and local safety regulations.1 Scope
37、This part of ISO 18254 describes analyses that are used to detect extractable alkylphenol ethoxylates (nonylphenol ethoxylates and octylphenol ethoxylates) in textile products. This document provides a method that uses Liquid Chromatograph (LC) with Mass Spectrometry (MS) system to detect and quanti
38、fy alkylphenol ethoxylates of defined ethoxylate chain length.2 PrincipleThe textile sample is cut into small pieces, transferred to a vial, and extracted with methanol using ultrasound. The extract is filtered and not subjected to any additional cleaning. Subsequently, the methanol extract is analy
39、sed by Liquid Chromatography (LC) with Mass Spectrometry (MS).3 ReagentsDuring the analysis, unless otherwise stated, only reagents of recognized analytical grade shall be used.NOTE OPEO and NPEO are available currently as technical grade.3.1 Solvents, of quality for HPLC analysis3.2 Octylphenol eth
40、oxylates, (Triton1)X-100), (OPEOs) CAS no. 9002-93-1, Sigma-Aldrich Part number T9284 (see Note in 3.3).3.3 Nonylphenol ethoxylates, (IGEPAL2)CO-630), (NPEOs) CAS no. 68412-54-4, Sigma-Aldrich Part number 542334 (see Note).NOTE The mentioned brand names in 3.2 and 3.3 are given to improve the compar
41、ability of the test results amongst laboratories. Using another batch or another supplier could lead to different results.3.4 Methanol.3.5 Acetonitrile (ACN).1) Triton is an example of a suitable product available commercially. This information is given for the convenience of users of this document
42、and does not constitute an endorsement by ISO of this product.2) IGEPAL is an example of a suitable product available commercially. This information is given for the convenience of users of this document and does not constitute an endorsement by ISO of this product.DIN EN ISO 18254-1:2016-09 EN ISO
43、18254-1:2016 (E)6 3.6 HPLC grade water.3.7 Formic acid, volume fraction of 30 %.3.8 Ammonium acetate.3.9 10 mM ammonium acetate, pH 3,6.3.9.1 0,771 g of ammonium acetate is dissolved in 900 ml of water (3.6).3.9.2 10 ml of ACN (3.5) is added and mixed well.3.9.3 The pH is adjusted to 3,6 with volume
44、 fraction of 30 % formic acid and made up to the mark with water (3.6) in a 1 l volumetric flask.3.9.4 The buffered solution should be filtered before use.4 Apparatus4.1 Apparatus and auxiliaries for preparing the sample4.1.1 Standard laboratory equipment.4.1.2 Analytical balance, resolution at 0,01
45、 g, for test specimen preparation.4.1.3 Analytical balance, resolution at 0,001 g, for standard preparation.4.1.4 Glass container with screw top, 40 ml has been found suitable.4.1.5 Ultrasonic water bath, to be set up at 70 C 5 C.4.1.6 Membrane filter, with 0,45 m pore size.4.1.7 Glass vial, with se
46、ptum cap (HPLC vial).4.1.8 pH meter, resolution of 0,1 pH.4.2 Chromatographic equipment4.2.1 High-performance Liquid Chromatography (LC) with Mass Spectrometry (MS) and Electro Spray Ionization (ESI).4.2.2 Reverse phase column with guard column.5 Procedure5.1 Standard preparationStock solutions of a
47、) OPEO and b) NPEO are prepared in methanol containing 1 000 mg/l OPEO (3.2) and NPEO (3.3).DIN EN ISO 18254-1:2016-09 EN ISO 18254-1:2016 (E)7 5.2 Sample preparationCut the textile sample into pieces of approximately 5 mm 5 mm and mix them homogeneously.Prepare approximately 1 g of the cut textile,
48、 weigh it to the nearest 10 mg, and then place it into the glass container (extraction vessel).Pipette 20 ml of methanol into the glass container (extraction vessel).Place the glass container (extraction vessel) into an ultrasonic bath at 70 C for (60 5) min.Afterwards, let the extract cool down to room temperature.Filter about 1 ml of the extraction solutio
