1、February 2016 English price group 9No 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-“2414810www.din.de
2、DIN EN 16711-2Textiles Determination of metal content Part 2: Determination of metals extracted by acidic artificial perspiration solution;English version EN 16711-2:2015,English translation of DIN EN 16711-2:2016-02Textilien Bestimmung des Metallgehaltes Teil 2: Bestimmung von extrahierbaren Metall
3、en mit saurer synthetischer Schweilsung;Englische Fassung EN 16711-2:2015,Englische bersetzung von DIN EN 16711-2:2016-02Textiles Dtermination de la teneur en mtaux Partie 2: Dosage des mtaux extraits au moyen dune solution de sueur artificielle acide;Version anglaise EN 16711-2:2015,Traduction angl
4、aise de DIN EN 16711-2:2016-02www.beuth.deDocument comprises 1 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.3 03.16DIN EN 16711-2:2016-02 2 A comma is used as the decimal marker. National foreword This document (EN 16711-2:2
5、015) has been prepared by Technical Committee CEN/TC 248 “Textiles and textile 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 T
6、extilchemische Prfverfahren und Fasertrennung. The DIN Standards corresponding 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
7、 3696 ISO 5725-1 DIN ISO 5725-1 ISO 5725-4 DIN ISO 5725-4 National Annex NA (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
8、definitions DIN ISO 5725-4, Accuracy (trueness and precision) of measurement 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 16711-2 November 2015 ICS 59.060.01 English Version Texti
9、les - Determination of metal content - Part 2: Determination of metals extracted by acidic artificial perspiration solution Textiles - Dtermination de la teneur en mtaux - Partie 2: Dosage des mtaux extraits au moyen dune solution de sueur artificielle acide Textilien - Bestimmung von Metallen - Tei
10、l 2: Bestimmung von extrahierbaren Metallen mit saurer synthetischer Schweilsung 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
11、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 versions (English, French, German). A
12、 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, Belgium, Bulgaria, Croatia, Cypr
13、us, 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 United Kin
14、gdom. EUROPEAN COMMITTEE FOR 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-
15、2:2015 EEN 16711-2:2015 (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 7 Procedure. 6 7.1 Extraction . 6 7.2 Determination of metals . 6 7.3 Reporting of results 6 8 Reliability of the method 6
16、9 Test report . 7 Annex A (informative) Reliability of the method 8 A.1 Trueness complying with ISO 5725-4 8 A.2 System precision . 9 A.3 Limit of detection and limit of quantification . 9 Annex B (informative) Extraction recovery. 10 Bibliography . 11 DIN EN 16711-2:2016 -02 EN 16711-2:2015 (E) 3 E
17、uropean foreword This document (EN 16711-2:2015) 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 end
18、orsement, 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
19、 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
20、 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, Irela
21、nd, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 16711-2:2016 -02 EN 16711-2:2015 (E) 4 1 Scope This European Standard specifies a procedure for determination of anti
22、mony (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 extraction with acidic artificial perspiration solution. 2 Normative
23、 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) appl
24、ies. EN 1233, Water quality Determination of chromium Atomic absorption spectrometric methods EN ISO 105-E04, Textiles Tests for colour fastness Part E04: Colour fastness to perspiration (ISO 105-E04) EN ISO 3071, Textiles Determination of pH of aqueous extract (ISO 3071) EN ISO 3696, Water for anal
25、ytical 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 spectro
26、metry (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: Determinat
27、ion 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 For determ
28、ination of soluble metals, the textile specimen is cut into small pieces and is extracted with acidic artificial perspiration solution. Analysis is performed with appropriate analytical techniques of atomic absorption and mass spectrometry (e.g. ICP-MS, ICP-OES, AAS, cold vapour atomic absorption sp
29、ectrometry, etc.). 4 Apparatus General laboratory equipment for analytical chemistry. In addition, the following is required: 4.1 Analytical balance, readability 0,000 1 g. DIN EN 16711-2:2016 -02 EN 16711-2:2015 (E) 5 4.2 Erlenmeyer flask (100 ml) with stopper or other appropriate closable vessel.
30、4.3 pH meter with glass electrode according to EN ISO 3071. 4.4 Shaker, optional horizontal or circular shaker. 4.5 Heating source (37 2) C, e.g. water bath. 4.6 Filter, pore size of 0,45 m. 5 Reagents Unless otherwise specified, analytical grade chemicals shall be used. 5.1 Perspiration solution co
31、mplying with EN ISO 105-E04. Dissolve with water (5.4) in a 1 000 ml flask: 0,5 g L-histidine-monohydrochloride-1-hydrate; 5,0 g sodium chloride; 2,2 g sodium dihydrogenphosphate-2-hydrate. Adjust the solution with diluted sodium hydroxide (5.3) or diluted hydrochloric acid (5.2) to pH (5,5 0,2). Ve
32、rify the compliance of the pH value using a pH electrode. Subsequently fill up with water (5.4) to the mark and homogenize the solution. 5.2 Hydrochloric acid, c(HCl) = 1 mol/l. 5.3 Sodium hydroxide, c(NaOH) = 1 mol/l. 5.4 Grade 2 water, complying with EN ISO 3696. 5.5 Metal standard solutions for c
33、alibration 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. 5.6 Nitric acid, (HNO3) = 65 %. 5.7 Dilution solution, 1,2 ml nitric acid (5.6) is diluted with water (5.4) to 100 ml. 6 Test specimen sampling Cut from th
34、e specimen, with a sharp pair of scissors made of noncorrosive material (preferably of ceramics) a representative sub-sample of approximately 1 g and record the mass to the nearest 0,1 mg. If the textile article is composed of several parts of products, such as knitted cuffs or lining, all kinds of
35、materials have to be tested as a representative composite sample with equal parts of the materials. Select the number of parts that can be collected as a composite sample, in correlation with the detection and quantification limits of the instrumental equipment. Weigh out materials, which cannot be
36、separated, as a composite sample. Consider also different colours of the material for sampling. Avoid any contact with metal articles, especially in wet conditions or with corrosive surfaces. DIN EN 16711-2:2016 -02 EN 16711-2:2015 (E) 6 7 Procedure 7.1 Extraction If there is sufficient test materia
37、l duplicate determinations shall be carried out. Approximately 1 g of the specimen is cut into small pieces (about 1 cm2) and the mass recorded to the nearest 0,1 mg), in order to ensure sufficient wetting, and is transferred into a Erlenmeyer flask or other contamination free vessels. For any mater
38、ials except felt and wool use 100 ml vessels. In the case of felt and wool use 250 ml vessels. Add 50 ml of acid synthetic perspiration solution (5.1) to the test specimen and stopper. The specimen is shaken briefly by hand in order to ensure a complete wetting of the textile sample. Subsequently, t
39、he specimen is shaken for 1 h at (37 2) C. The shaking frequency is adjusted to 60 cycles per minute in case of a horizontal shaker and to 30 cycles per minute using a circular shaker. Alternatively, stirring with a magnetic stirrer is allowed. Subsequently, filter (4.6) the extract in order to remo
40、ve small textile particles and fluff. 7.2 Determination of metals Determination of the metal amounts in the digestion solutions is performed complying with EN 1233, EN ISO 11885, EN ISO 12846, EN ISO 15586, EN ISO 17294-2, EN ISO 17852 or ISO 8288. Calibration is performed either with calibration so
41、lutions in the appropriate matrix or via standard addition. In the case of excessive concentrations, the test solutions may be diluted with dilution solution (5.7) depending on the analytical system. 7.3 Reporting of results The metal contents in the textile have to be specified in milligram per kil
42、ogram (mg/kg). The results of 7.2 are calculated according to the following equation: )1000()(=mVd where d metal content as mass portion, in milligrams per kilogram (mg/kg); mass concentration of metal in the extraction solution, in micrograms per litre (g/l); V volume of solvent, in millilitres (ml
43、); m weight of specimen, in grams (g). If a dilution has been applied for testing, the dilution factor has to be taken into account for the determination of the result. 8 Reliability of the method The results of the round robin test can be found in Annex A. NOTE “Trueness” and “precision” are terms
44、complying with ISO 5725-1 to describe the accuracy of test methods. DIN EN 16711-2:2016 -02 EN 16711-2:2015 (E) 7 9 Test report The test report shall state at least the following particulars: a) name of the laboratory; b) reference to this European Standard; c) specification of the applied analytica
45、l system; d) specification of the specimen; e) amount of each targeted metal in mg/kg; f) any discrepancy from this European Standard, if relevant. DIN EN 16711-2:2016 -02 EN 16711-2:2015 (E) 8 Annex A (informative) Reliability of the method A.1 Trueness complying with ISO 5725-4 “Trueness” refers t
46、o the closeness of agreement between the arithmetic mean of a large number of test results and the true or accepted reference value. Trueness was calculated as systematic measurement error (bias) of the method and in correlation to the mean value, because no reference value of the investigated mater
47、ial is available. In a round robin test 2006 of NMP a textile specimen was tested for metal content using different test methods. The measured values of the participating laboratories deviated partly from each other. For result evaluation particular laboratory values (“outliers”) were eliminated res
48、ulting in good correlation based on the calculation of standard deviation. Calculation of mean value and standard deviation after elimination of deviating values (marked in grey) for the determination of metals after extraction with acid synthetic perspiration solution. Table A.1 Results of statisti
49、cal evaluation: Determination of contents after extraction with perspiration solution Metal Metal content mg/kg Mean value x mg/kg Standard deviation s mg/kg Variation coefficient v % Laboratory A B C D E F G H Sb 4,59 6,50 6,27 6,77 5,54 7,80 4,30 5,11 5,86 1,189 20 As 0,60 10 0,46 0,42 0,53 0,45 0,73 0,59 0,54 0,109 20 Pb 0,48 0,30 0,89 0,48 0,44 0,48 0,59 0,96 0,58 0,230 40 Cd 0,07 0,20 0,16 0,20 0,17 0,17 0,17 0,20 0,18 0,018 10 Cr 2,90 2,00 2,94 2,31 2,39 2,91 2,90 3,14 2,69 0,399 15 C
