SIST EN 16711-1:2016

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.DERTextilien - Bestimmung von Metallen - Teil 1: Bestimmung von Metallen mittels MikrowellenaufschlussTextiles - Détermination de la teneur en métaux - Partie 1: Dosage des métaux par minéralisation par micro-ondesTextiles - Determination of metal content - Part 1: Determination of metals using microwave digestion59.060.01Tekstilna vlakna na splošnoTextile fibres in generalICS:Ta slovenski standard je istoveten z:EN 16711-1:2015SIST EN 16711-1:2016en,fr,de01-januar-2016SIST EN 16711-1:2016SLOVENSKI
STANDARD



SIST EN 16711-1:2016



EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 16711-1
November
t r s w ICS
w {ä r x rä r s English Version
Textiles æ Determination of metal content æ Part
sã Determination of metals using microwave digestion Textiles æ Détermination de la teneur en métaux æ Partie
sã Dosage des métaux par minéralisation par microæondes
Textilien æ Bestimmung von Metallen æ Teil
sã Bestimmung von Metallen mittels Mikrowellenaufschluss This European Standard was approved by CEN on
w September
t r s wä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey andUnited Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Avenue Marnix 17,
B-1000 Brussels
9
t r s w CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s x y s sæ sã t r s w ESIST EN 16711-1:2016



EN 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 . 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 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 . 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.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
SIST EN 16711-1:2016



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 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. 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. 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 solution. 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, 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. SIST EN 16711-1:2016



EN 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), nickel (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. 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 — Specification 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 without 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 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 determined 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 chemistry. 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). SIST EN 16711-1:2016



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) = 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 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 specimen (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 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 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 paint 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 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 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 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 children’s 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 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. SIST EN 16711-1:2016



EN 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, concentrated 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 analysing 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 ce
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