1、BSI Standards PublicationBS EN ISO 18254-1:2016Textiles Method for thedetection and determination ofalkylphenol ethoxylates (APEO)Part 1: Method using HPLC MS (ISO18254-1:2016)BS EN ISO 18254-1:2016 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO18254-1:2016
2、.The UK participation in its preparation was entrusted to TechnicalCommittee TCI/80, Chemical testing of textiles.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. U
3、sers are responsible for its correctapplication. The British Standards Institution 2016. Published by BSI StandardsLimited 2016ISBN 978 0 580 93757 6ICS 59.080.01Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of
4、 theStandards Policy and Strategy Committee on 31 May 2016.Amendments issued since publicationDate Text affectedEUROPEAN 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 (
5、APEO) - Part 1: Method using HPLC - MS (ISO 18254-1:2016) Textiles - Mthode de dtection 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
6、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 on application to the CEN-CENELEC Management
7、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-CENELEC Management Centre has the same status as
8、 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, Italy, Latvia, Lithuania, Luxembourg, Malta, Net
9、herlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, 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 ri
10、ghts of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 18254-1:2016 EBS EN ISO 18254-1:2016EN ISO 18254-1:2016 (E) 3 European foreword This document (EN ISO 18254-1:2016) has been prepared by Technical Committee ISO/TC 38 “Textiles“ in collabor
11、ation 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, at the latest by October 2016, and conflicting nat
12、ional 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 be held responsible for identifying any or all such patent rights. According to the CEN
13、-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, Hungar
14、y, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 18254-1:2016 has been approved by CEN as EN ISO 18254-1:2016 without any
15、 modification. BS EN ISO 18254-1:2016ISO 18254-1:2016(E)Foreword ivIntroduction v1 Scope . 12 Principle 13 Reagents 14 Apparatus . 24.1 Apparatus and auxiliaries for preparing the sample . 24.2 Chromatographic equipment . 25 Procedure. 25.1 Standard preparation 25.2 Sample preparation 35.3 Analysis
16、36 Calculation of results . 36.1 Determination of the R value for each congener of APEO . 36.2 Calibration curve . 36.3 Calculation of concentration of APEO result . 47 Test report . 4Annex A (informative) Examples of chromatographic method LC/MS . 5Annex B (informative) Examples of chromatographic
17、method LC/MS/MS 8Bibliography .10 ISO 2016 All rights reserved iiiContents PageBS EN ISO 18254-1:2016ISO 18254-1:2016(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Sta
18、ndards 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-governmental, in liaison with ISO, also
19、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 the ISO/IEC Directives, Part 1. In
20、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 possibility that some of the elements
21、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 patent declarations received (se
22、e 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 information about ISOs adherence t
23、o 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, and Technical Committee CEN/TC 248
24、, 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 ethoxylates (APEO): Part 1: Method usi
25、ng HPLC-MSThe following part is under preparation: Part 2; Method using NPLCiv ISO 2016 All rights reservedBS EN ISO 18254-1:2016ISO 18254-1:2016(E)IntroductionAlkylphenol ethoxylates (APEOs) are high-value products commonly used in industrial and consumer detergents and cleaners, some plastics and
26、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 species, minimi
27、zation 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 to biodegrad
28、e. 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 nonylphenol ethoxylate
29、s 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, which repealed
30、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. ISO 2016 All rights reserved vBS EN ISO 18254-1:2016BS EN ISO 18254-1:2016Textiles Method for the detection and determ
31、ination of alkylphenol ethoxylates (APEO) Part 1: Method using HPLC-MSSAFETY PRECAUTIONS It is the users responsibility to use safe and proper techniques in handling materials in this test method. Consult manufacturers for specific details such as material safety, data sheets, and other recommendati
32、ons. Good laboratory practice should be followed. Users should comply with any national and local safety regulations.1 ScopeThis part of ISO 18254 describes analyses that are used to detect extractable alkylphenol ethoxylates (nonylphenol ethoxylates and octylphenol ethoxylates) in textile products.
33、 This document provides a method that uses Liquid Chromatograph (LC) with Mass Spectrometry (MS) system to detect and quantify 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 u
34、ltrasound. The extract is filtered and not subjected to any additional cleaning. Subsequently, the methanol extract is analysed by Liquid Chromatography (LC) with Mass Spectrometry (MS).3 ReagentsDuring the analysis, unless otherwise stated, only reagents of recognized analytical grade shall be used
35、.NOTE OPEO and NPEO are available currently as technical grade.3.1 Solvents, of quality for HPLC analysis3.2 Octylphenol ethoxylates, (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-
36、4, Sigma-Aldrich Part number 542334 (see Note).NOTE The mentioned brand names in 3.2 and 3.3 are given to improve the comparability 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 ex
37、ample 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.2) IGEPAL is an example of a suitable product available commercially. This information is given for the convenienc
38、e of users of this document and does not constitute an endorsement by ISO of this product.INTERNATIONAL STANDARD ISO 18254-1:2016(E) ISO 2016 All rights reserved 1BS EN ISO 18254-1:2016ISO 18254-1:2016(E)3.6 HPLC grade water.3.7 Formic acid, volume fraction of 30 %.3.8 Ammonium acetate.3.9 10 mM amm
39、onium 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 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 buffere
40、d 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 g, for test specimen preparation.4.1.3 Analytical balance, resolution at 0,001 g, for standard preparation.4.1.4
41、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 septum cap (HPLC vial).4.1.8 pH meter, resolution of 0,1 pH.4.2 Chromatographic equipment4.2.1 High-performance Liqu
42、id 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) OPEO and b) NPEO are prepared in methanol containing 1 000 mg/l OPEO (3.2) and NPEO (3.3).2 ISO 2016 All rights
43、reservedBS EN ISO 18254-1:2016ISO 18254-1:2016(E)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, weigh it to the nearest 10 mg, and then place it into the glass container (extraction vessel).
44、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 solution into a HPLC vial using a disposab
45、le syringe equipped with a membrane filter.5.3 AnalysisThe detection and quantification of defined alkylphenol ethoxylates is conducted using LC/MS with gradient elution and ESI mass spectrometer.Congeners with 2 to 16 ethoxylate groups shall be used for quantification.Guidelines for suitable chroma
46、tographic conditions are given in Annex A for LC/MS and in Annex B for LC/MS/MS.6 Calculation of results6.1 Determination of the R value for each congener of APEOCalibrate the mass fraction (R) for each APEO congener and calculate the concentration of each APEO isomer as follows.A mass fraction in e
47、ach APEO (n), R (%)AOAOT100= (1)whereAO is the area response of each APEO congener;AOT is the total sum of APEO area responses (from APEO 2 to APEO 16).Exact concentration in each APEO (n), Exact concentration (mg/l) 100std=RCmg/l (2)whereCstdis the concentration of APEO standard mix solution of eac
48、h working solution.6.2 Calibration curveCalibration curves with standards of a) OPEO and b) NPEO at 0,5 mg/l, 2 mg/l, and 5 mg/l are prepared with at least three calibration points.NOTE Concentration ranges for the calibration standards are subject to change upon the need of each laboratory and equi
49、pment used.For quantification, the calibration curve shall have a correlation coefficient greater than 0,990 (R2greater than 0,995). ISO 2016 All rights reserved 3BS EN ISO 18254-1:2016ISO 18254-1:2016(E)6.3 Calculation of concentration of APEO resultThe APEO level in the textile sample is calculated according to Formula (3).NPEOs in sample, NPEOs (mg/kg)=CVMDF (3)whereCis the total sum of concentration of each NPEO isomer (mg/l), with: CRii=NPEO ;i represents the ethoxylate chain length;Riis the percentage o
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