1、February 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 59.060.01!%LS.“2414811www.din.d
2、eDIN EN 16711-1Textiles Determination of metal content Part 1: Determination of metals using microwave digestion;English version EN 16711-1:2015,English translation of DIN EN 16711-1:2016-02Textilien Bestimmung des Metallgehaltes Teil 1: Bestimmung von Metallen mittels Mikrowellenaufschluss;Englisch
3、e Fassung EN 16711-1:2015,Englische bersetzung von DIN EN 16711-1:2016-02Textiles Dtermination de la teneur en mtaux Partie 1: Dosage des mtaux par minralisation par micro-ondes;Version anglaise EN 16711-1:2015,Traduction anglaise de DIN EN 16711-1:2016-02www.beuth.deDocument comprises 16 pagesDTran
4、slation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.03.16DIN EN 16711-1:2016-02 2 A comma is used as the decimal marker. National foreword This document (EN 16711-1:2015) has been prepared by Technical Committee CEN/TC 248 “Textiles and text
5、ile products” (Secretariat: BSI, United Kingdom). The responsible German body involved in its preparation was DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing), Working Committee NA 062-05-12 AA Textilchemische Prfverfahren und Fasertrennung. The DIN Standards correspond
6、ing to the International Standards referred to in this document are as follows, whereby EN ISO Standards are only listed below if these have not been published as DIN EN ISO Standards with the same number: EN ISO 3696 DIN ISO 3696 ISO 5725-1 DIN ISO 5725-1 ISO 5725-4 DIN ISO 5725-4 National Annex NA
7、 (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods DIN ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-4, Accuracy (trueness and precision) of measuremen
8、t methods and results Part 4: Basic methods for the determination of the trueness of a standard measurement method EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16711-1 November 2015 ICS 59.060.01 English Version Textiles - Determination of metal content - Part 1: Determination of metals usin
9、g microwave digestion Textiles - Dtermination de la teneur en mtaux - Partie 1: Dosage des mtaux par minralisation par micro-ondes Textilien - Bestimmung von Metallen - Teil 1: Bestimmung von Metallen mittels Mikrowellenaufschluss This European Standard was approved by CEN on 5 September 2015. CEN m
10、embers 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 on applic
11、ation 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-CENELEC Mana
12、gement 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, Italy, Latvi
13、a, Lithuania, Luxembourg, Malta, Netherlands, 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
14、 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 16711-1:2015 EEN 16711-1:2015 (E) 2 Contents Page European foreword . 3 1 Scope 4 2 Normative references 4 3 Principle . 4 4 Apparatus . 4 5 Reagents . 5 6 T
15、est specimen sampling . 5 6.1 Natural and man-made textiles 5 6.2 Garment components with painted and other similar surface coatings . 5 6.3 Metallic products . 5 6.4 Non-metal products 6 6.4.1 General 6 6.4.2 Ceramics, glass and crystal and other siliceous materials . 6 6.4.3 Plastics, polymers ( i
16、ncludes prints and coatings other than 6.2) and other non- siliceous materials 6 7 Procedure. 6 7.1 Digestion of natural and man-made textiles, and coated fabrics 6 7.2 Digestion of paint and other similar surface coatings . 6 7.3 Digestion of metallic products 7 7.4 Digestion of non-metal products
17、. 7 7.4.1 Ceramics, glass and crystal and other siliceous materials . 7 7.4.2 Plastics, polymers and other non-siliceous materials . 8 7.5 Determination of metals . 8 7.6 Reporting of results 8 8 Reliability of the method 9 9 Test report . 9 Annex A (informative) Laboratory microwave procedure 10 A.
18、1 Cleaning of polytetrafluoroethylene glassware and vessels 10 A.2 Sample preparation (digestion) . 10 Annex B (informative) Procedure characteristics 12 B.1 Trueness complying with ISO 5725-4 . 12 B.2 System precision 13 B.3 Limit of detection and limit of quantification 13 Bibliography . 14 DIN EN
19、 16711-1:2016 -02 EN 16711-1:2015 (E) 3 European foreword This document (EN 16711-1:2015) has been prepared by 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 p
20、ublication of an identical text or by endorsement, at the latest by May 2016, and conflicting national standards shall be withdrawn at the latest by May 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 shal
21、l not be held responsible for identifying any or all such patent rights. EN 16711, Textiles Determination of metal content is composed of the following parts: Part 1: Determination of metals using microwave digestion; Part 2: Determination of metals extracted by acidic artificial perspiration soluti
22、on. 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, Estonia, Finland, Former Yugoslav Republic of Macedonia, France,
23、 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. DIN EN 16711-1:2016 -02 EN 16711-1:2015 (E) 4 1 Scope This European Standard specif
24、ies a procedure for determination of metals, in particular antimony (Sb), arsenic (As), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), lead (Pb), mercury (Hg), nickel (Ni) in natural and man-made textiles, including coated fabrics and garment components (e.g. buttons, zips, etc.) after micro
25、wave digestion. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (inc
26、luding any amendments) applies. EN 1233, Water quality Determination of chromium Atomic absorption spectrometric methods EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) EN ISO 11885, Water quality Determination of selected elements by inductively coupled pl
27、asma optical emission spectrometry (ICP-OES) (ISO 11885) EN ISO 12846, Water quality Determination of mercury Method using atomic absorption spectrometry (AAS) with and without enrichment (ISO 12846) EN ISO 15586, Water quality Determination of trace elements using atomic absorption spectrometry wit
28、h graphite furnace (ISO 15586) EN ISO 17294-2, Water quality Application of inductively coupled plasma mass spectrometry (ICP-MS) Part 2: Determination of 62 elements (ISO 17294-2) EN ISO 17852, Water quality Determination of mercury Method using atomic fluorescence spectrometry (ISO 17852) ISO 8288
29、, Water quality Determination of cobalt, nickel, copper, zinc, cadmium and lead Flame atomic absorption spectrometric methods 3 Principle The total metal content is determined after microwave digestion. Analysis is performed with appropriate analytical techniques of atomic absorption, inductively co
30、upled plasma and mass spectrometry (e.g. ICP-MS, ICP-OES, AAS, cold vapor atomic absorption spectrometry, etc.). 4 Apparatus General laboratory equipment for analytical chemistry. In addition, the following is required: 4.1 Analytical balance, readability 0,000 1 g. 4.2 Microwave digestion system wi
31、th appropriate high pressure vessels. 4.3 Appropriate digestion vessels, e.g. of polytetrafluoroethylene (PTFE). DIN EN 16711-1:2016 -02 EN 16711-1:2015 (E) 5 5 Reagents Unless otherwise specified, analytical grade chemicals shall be used. 5.1 Nitric acid, (HNO3) = 65 %. 5.2 Sulphuric acid, (H2SO4)
32、= 96 %. 5.3 Hydrofluoric acid, (HF) = 48 %. 5.4 Grade 2 water, complying with EN ISO 3696. 5.5 Hydrogen peroxide, (H2O2) = 30 %. 5.6 Metal standard solutions for calibration of the analytical systems complying with EN 1233, EN ISO 11885, EN ISO 12846, EN ISO 15586, EN ISO 17294-2, EN ISO 17852 or IS
33、O 8288. 5.7 Dilution solution, 1,2 ml nitric acid (5.1) is made up to 100 ml with water (5.4). 6 Test specimen sampling 6.1 Natural and man-made textiles Cut from the textile specimen (with a sharp pair of scissors made of noncorrosive material, preferably of ceramics) a representative subsample of
34、approximately 0,5 g and record the mass to the nearest 0,1 mg. If the textile article is composed of several parts of textile products, such as knitted cuffs or lining, all the different types of materials have to be tested as a representative composite specimen with equal parts of each component. S
35、elect the number of parts that can be collected as a composite specimen in relation to the detection and quantification limits of the instrumental equipment. Weigh out materials that cannot be separated as one specimen. Consider also different colours of the material for sampling. Avoid any contact
36、with metal articles, especially in wet conditions or with corrosive surfaces. 6.2 Garment components with painted and other similar surface coatings For products coated with paint or a similar surface coating, remove and digest the coating separately from the substrate material. Care should be taken
37、 to remove as little of the substrate as possible. It may be necessary to add a few drops of a solvent, such as dichloromethane, to soften the paint and aid in its removal from the substrate. If used, such solvent shall be evaporated fully prior to analysis. The scraped paint shall be finely divided
38、 to help in the digestion. Scrape approximately 100 mg to 200 mg of paint from the product. If it is not possible to collect this much paint it may be necessary to combine more than one unit of such product to collect sufficient paint. 6.3 Metallic products When preparing a sample, the laboratory sh
39、all make every effort to assure that the aliquot removed from a component part of a sample is representative of the component to be tested, and is free of contamination. If the item is coated with paint or a similar surface coating, the coating shall be removed and analysed, separately from the base
40、 metal, for metal content as described in 6.2. Component parts of childrens products, including metal jewellery items, generally weigh several grams or more, and an aliquot (with no paint or similar surface coating) will have to be obtained. Samples should be cut or ground into many small pieces to
41、increase the rate of dissolution. If used, grinding apparatus (such as a rotary grinding tool with disposable grinding bits) must be thoroughly cleaned to prevent cross-contamination. DIN EN 16711-1:2016 -02 EN 16711-1:2015 (E) 6 6.4 Non-metal products 6.4.1 General The general approach is to grind
42、or cut any accessible component part of a sample into small pieces or a powder; digest an aliquot completely in nitric acid or, for siliceous products, in a combination of hot, concentrated nitric and hydrofluoric acids. 6.4.2 Ceramics, glass and crystal and other siliceous materials Ceramic items g
43、enerally weigh several grams or more, and consist of the base ceramic with a glaze and decoration fired on. The metals in ceramics are generally in the glaze or decoration. When analysing ceramics or glass, the entire item including the glaze, decoration, and ceramic base material should be ground i
44、n a cryogenic mill and 100 mg to 200 mg of the ground ceramic/glass powder weighed in an appropriate microwave vessel. If used, the grinding apparatus must be thoroughly cleaned to prevent cross-contamination. 6.4.3 Plastics, polymers ( includes prints and coatings other than 6.2) and other non- sil
45、iceous materials Cut the test specimen into small pieces. Hard to digest plastics may need to be cryomilled to get a finer powder. Ensure the milling apparatus is thoroughly clean between test specimens to avoid cross-contamination. 7 Procedure 7.1 Digestion of natural and man-made textiles, and coa
46、ted fabrics Perform a microwave digestion using a mixture of nitric acid and hydrogen peroxide, examples are given in Annex A. Other digestion methods may be used if the same results are obtained. Weigh out 0,1 g to 0,5 g of the finely cut specimen (record the mass to the nearest 0,1 mg) and put int
47、o a clean PTFE vessel. Add 4 ml of water (5.4) for surface wetting and subsequently 10 ml nitric acid (5.1) and 4 ml hydrogen peroxide (5.5) (see Table A.3) or 8 ml nitric acid (5.1) and 2,5 ml hydrogen peroxide (5.5) (see Table A.4). Care shall be taken to ensure that the specimen is wetted with ac
48、id, since otherwise burning of the sample material may occur. The filled volume of the PTFE vessels should not exceed 30 % to 40 % of the total volume. Residues resulting from pigments or admixtures of titanium oxide in polyester and polyamide fibres have to be removed by filtration. 7.2 Digestion o
49、f paint and other similar surface coatings Weigh 0,1 g to 0,2 g (record the mass to the nearest 0,1 mg) of the paint into a clean liner of the microwave digestion vessel. Carefully add at least 5 ml of concentrated nitric acid or extraction solution (made with 60 ml HNO3 conc and 180 ml HCl conc / 1 l water grade 2. Prepare also a digestion blank with the samples. Use a certified reference material if available (e.g. such as NIST SRM 2581 or 2582 for lead determination) to control the digestion. The result should be
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