1、BSI Standards PublicationBS EN 16711-1:2015Textiles Determination ofmetal contentPart 1: Determination of metals usingmicrowave digestionIncorporating corrigendum November 2015BS EN 16711-1:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of EN 16711-1:2015.The UK
2、 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. Users ar
3、e responsible for its correctapplication. The British Standards Institution 2015. Published by BSI Standards Limited 2015ISBN 978 0 580 92482 8ICS 59.060.01Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theSt
4、andards Policy and Strategy Committee on 30 November 2015.Amendments/corrigenda issued since publicationDate Text affected30 November 2015 This corrigendum replaces the main text of thedocument with the correct standard BS EN 16711-1:2015EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 16711-1 N
5、ovember 2015 ICS 59.060.01 English Version Textiles - Determination of metal content - Part 1: Determination of metals using 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:
6、Bestimmung von Metallen mittels Mikrowellenaufschluss This European Standard was approved by CEN on 5 September 2015. 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 a
7、ny 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 versions (English, French, German). A version in any other langu
8、age 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, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark
9、, 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, Switzerland, Turkey andUnited Kingdom. EUROPEAN COMMITTEE FOR
10、 STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 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 EBS EN 16711-1:2015EN
11、 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 Test 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
12、. 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 ( includes 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 fabr
13、ics 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 . 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 met
14、als . 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.1 Cleaning of polytetrafluoroethylene glassware and vessels 10 A.2 Sample preparation (digestion) . 10 Annex B (informative) Procedure characteristics 12 B.1 T
15、rueness complying with ISO 5725-4 . 12 B.2 System precision 13 B.3 Limit of detection and limit of quantification 13 Bibliography . 14 BS EN 16711-1:2015EN 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 p
16、roducts”, 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 May 2016, and conflicting national standards shall be withdrawn at the latest by May 2016. Attent
17、ion 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. EN 16711, Textiles Determination of metal content is composed of the following parts: Part 1
18、: Determination of metals using microwave digestion; Part 2: Determination of metals extracted by acidic artificial perspiration solution. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard:
19、 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, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain,
20、Sweden, Switzerland, Turkey and the United Kingdom. BS EN 16711-1:2015EN 16711-1:2015 (E) 4 1 Scope This European Standard specifies a procedure for determination of metals, in particular antimony (Sb), arsenic (As), cadmium (Cd), chromium (Cr), cobalt (Co), copper (Cu), lead (Pb), mercury (Hg), nic
21、kel (Ni) in natural and man-made textiles, including coated fabrics and garment components (e.g. buttons, zips, etc.) after microwave digestion. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application.
22、 For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 1233, Water quality Determination of chromium Atomic absorption spectrometric methods EN ISO 3696, Water for analytical laboratory use S
23、pecification and test methods (ISO 3696) EN ISO 11885, Water quality Determination of selected elements by inductively coupled plasma optical emission spectrometry (ICP-OES) (ISO 11885) EN ISO 12846, Water quality Determination of mercury Method using atomic absorption spectrometry (AAS) with and wi
24、thout enrichment (ISO 12846) EN ISO 15586, Water quality Determination of trace elements using atomic absorption spectrometry with 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
25、 17294-2) EN ISO 17852, Water quality Determination of mercury Method using atomic fluorescence spectrometry (ISO 17852) ISO 8288, Water quality Determination of cobalt, nickel, copper, zinc, cadmium and lead Flame atomic absorption spectrometric methods 3 Principle The total metal content is determ
26、ined after microwave digestion. Analysis is performed with appropriate analytical techniques of atomic absorption, inductively coupled plasma and mass spectrometry (e.g. ICP-MS, ICP-OES, AAS, cold vapor atomic absorption spectrometry, etc.). 4 Apparatus General laboratory equipment for analytical ch
27、emistry. In addition, the following is required: 4.1 Analytical balance, readability 0,000 1 g. 4.2 Microwave digestion system with appropriate high pressure vessels. 4.3 Appropriate digestion vessels, e.g. of polytetrafluoroethylene (PTFE). BS EN 16711-1:2015EN 16711-1:2015 (E) 5 5 Reagents Unless
28、otherwise specified, analytical grade chemicals shall be used. 5.1 Nitric acid, (HNO3) = 65 %. 5.2 Sulphuric acid, (H2SO4) = 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
29、the analytical systems complying with EN 1233, EN ISO 11885, EN ISO 12846, EN ISO 15586, EN ISO 17294-2, EN ISO 17852 or ISO 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 sp
30、ecimen (with a sharp pair of scissors made of noncorrosive material, preferably of ceramics) a representative subsample of 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
31、different types of materials have to be tested as a representative composite specimen with equal parts of each component. Select 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
32、 that cannot be separated as one specimen. Consider also different colours of the material for sampling. Avoid any contact 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 pai
33、nt or a similar surface coating, remove and digest the coating separately from the substrate material. Care should be taken 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
34、the substrate. If used, such solvent shall be evaporated fully prior to analysis. The scraped paint shall be finely divided 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
35、than one unit of such product to collect sufficient paint. 6.3 Metallic products When preparing a sample, the laboratory shall 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
36、item is coated with paint or a similar surface coating, the coating shall be removed and analysed, separately from the base 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 (wit
37、h no paint or similar surface coating) will have to be obtained. Samples should be cut or ground into many small pieces to 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-contamin
38、ation. BS EN 16711-1:2015EN 16711-1:2015 (E) 6 6.4 Non-metal products 6.4.1 General The general approach is to grind 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, concen
39、trated nitric and hydrofluoric acids. 6.4.2 Ceramics, glass and crystal and other siliceous materials Ceramic items generally 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 analy
40、sing ceramics or glass, the entire item including the glaze, decoration, and ceramic base material should be ground in 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 pr
41、event cross-contamination. 6.4.3 Plastics, polymers ( includes prints and coatings other than 6.2) and other non- siliceous 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 bet
42、ween test specimens to avoid cross-contamination. 7 Procedure 7.1 Digestion of natural and man-made textiles, and coated 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
43、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 into 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)
44、and 2,5 ml hydrogen peroxide (5.5) (see Table A.4). Care shall be taken to ensure that the specimen is wetted with acid, 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 pigment
45、s or admixtures of titanium oxide in polyester and polyamide fibres have to be removed by filtration. 7.2 Digestion of 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 ad
46、d 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 contr
47、ol the digestion. The result should be between 15 % of the true value. Seal the vessels and load into the microwave oven according to the manufacturers instructions. Programme the microwave digestion system using a programme with enough temperature or power to digest the sample (check this with the
48、certified reference material). At the end of the digestion period, remove the vessels from the microwave oven, place them in a fume hood, and allow the solutions to cool to room temperature. BS EN 16711-1:2015EN 16711-1:2015 (E) 7 Carefully open the vessels (pay attention to the gas pressure that ma
49、y be present inside the vessels). Quantitatively transfer the liquid contents of each vessel to a 50 ml volumetric flask (the size may be adjusted and will depend on the required limit). Carefully rinse each vessel with grade 2 water into the volumetric flask and bring to volume with water (be sure that the liquid temperature is near room temperature before making the volume up to the mark) . Seal each volumetric flask with a stopper and mix thoroughly. 7.3 Digestion of metallic products Weigh out 0,1 g to 0,2 g (record the mass to the n
