1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 12149 : 1998 The Eu
2、ropean Standard EN 12149 : 1997 has the status of a British Standard ICS 91.180 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Wallcoverings in roll form Determination of migration of heavy metals and certain other elements, of vinyl chloride monomer and of formaldehyde relea
3、seThis British Standard, having been prepared under the direction of the Consumer Products and Services Sector Board, was published under the authority of the Standards Board and comes into effect on 15 February 1998 BSI 1998 ISBN 0 580 29508 7 BS EN 12149 : 1998 Amendments issued since publication
4、Amd. No. Date Text affected National foreword This British Standard reproduces verbatim EN 12149 : 1997 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee CW/35, Wallcoverings, which has the responsibility to: aid enquirers to
5、understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Cross-references The British Standards which imp
6、lement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled International Standards Correspondence Index, or by using the Find facility of the BSI Standards Electronic Catalogue. Compliance with a British Standard
7、does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, the EN title page, pages 2 to 12, an inside back cover and a back cover.BS EN 12149 : 1998 BSI 1998 i Contents Page Committees responsible Inside
8、front cover National foreword ii Foreword 2 Text of EN 12149 3blankCEN European Committee for Standardization Comite Europe en de Normalisation Europa isches Komitee fu r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1997 CEN All rights of exploitation in any form and by any means
9、 reserved worldwide for CEN national Members. Ref. No. EN 12149 : 1997 E EUROPEAN STANDARD EN 12149 NORME EUROPE ENNE EUROPA ISCHE NORM October 1997 ICS 91.180 Descriptors: Wall coverings, wall paper base, plastic coatings, tests, determination of content, metals, migrations, formaldehyde, vinyl chl
10、oride English version Wallcoverings in roll form Determination of migration of heavy metals and certain other elements, of vinyl chloride monomer and of formaldehyde release Reve tements muraux en rouleaux De termination de la migration de me taux lourds et certains autres e le ments extractibles, d
11、e la teneur en chlorure de vinyle monome re et du de gagement de formalde hyde Wandbekleidungen in Rollen - Bestimmung der Migration von Schwermetallen und bestimmten anderen extrahierenden Elementen, des Gehaltes an Vinylchlorid Monomer sowie an Formaldehydabgabe This European Standard was approved
12、 by CEN on 3 August 1997. 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 any alteration. Up-to-date lists and bibliographical references concerning such national stan
13、dards may be obtained on application to the Central Secretariat 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
14、 the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and Unit
15、ed Kingdom.Page 2 EN 12149 : 1997 BSI 1998 Foreword This European Standard has been prepared by Technical Committee CEN/TC 99, Wallcoverings, of which the secretariat is held by BSI. The following other European standards exist relating to wallcoverings: EN 233 : 1989 (+A1 : 1996) Wallcoverings in r
16、oll form Specification for finished wallpapers, wall vinyls and plastics wallcoverings EN 234 : 1989 (+A1 : 1996) Wallcoverings in roll form Specification for wallcoverings for subsequent decoration EN 235 : 1989 Wallcoverings in roll form Vocabulary and symbols EN 259 : 1992 (+A1 : 1996) Wallcoveri
17、ngs in roll form Specification for heavy duty wallcoverings EN 266 : 1992 Textile wallcoverings 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 April 1998, and conflicting national standards shall
18、 be withdrawn at the latest by April 1998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland,
19、Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Contents Page Foreword 2 Introduction 3 1 Scope 3 2 Normative references 3 3 Definitions 3 4 Test A: Migration of heavy metals and certain other elements (antimony, arsenic, barium, cadmium, chromium
20、, mercury, lead and selenium) 3 5 Test B: Determination of vinyl chloride monomer 5 6 Test C: Determination of formaldehyde using the modified WKl method 7 7 Test report 10 Annex A (informative) Bibliography 12Page 3 EN 12149 : 1997 BSI 1998 Introduction This European standard has been prepared to c
21、over factors which are considered to be environmental requirements of wallcoverings. The methods of test are based on those described in standards and published work as given in annex A. 1 Scope This European standard specifies three methods of test concerning respectively: test A: the migration of
22、heavy metals and certain other elements (antimony, arsenic, barium, cadmium, chromium, mercury, lead and selenium); test B: the determination of vinyl chloride monomer; test C: the determination of formaldehyde release. This European Standard applies to all wallcoverings in roll form. 2 Normative re
23、ferences This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of
24、these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest editions of the publication referred to applies. EN 235 Wallcoverings in roll form Vocabulary and symbols EN ISO 3696 Water for analytical laboratory use Specif
25、ication and test methods (ISO 3696:1987) ISO 187 Paper, board and pulps Standard atmosphere for conditioning and testing and procedure for monitoring the atmosphere and conditioning of samples 3 Definitions For the purposes of this European standard, the definitions given in EN 235 apply. 4 Test A:
26、Migration of heavy metals and certain other elements (antimony, arsenic, barium, cadmium, chromium, mercury, lead and selenium) 4.1 Principle The soluble elements are extracted under conditions simulating the ingestion of the materials. The content present in the extract is then determined. 4.2 Reag
27、ents 4.2.1 During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and water of equivalent purity to grade 3 according to EN ISO 3696. 4.2.2 Hydrochloric acid solution (0,07 0,005) mol/l. 4.2.3 Hydrochloric acid solution (2 0,1) mol/l. 4.3 Test apparatus 4.3.1
28、Usual laboratory apparatus and glassware. 4.3.2 pH meter, having an accuracy of 0,2 pH units. 4.3.3 Shaker, capable of producing a linear reciprocating movement of an amplitude of (2 0,5) cm with a frequency of 1 Hz. 4.3.4 Oven, capable of maintaining a constant temperature of (37 2) C. 4.3.5 Filter
29、, with a pore size of 0,45mm. 4.4 Test specimens 4.4.1 Preparation of test specimens 4.4.1.1 Roll (except borders) Take a roll of wallcovering and make two cuts across the width of the wallcovering to produce a strip (30 1) mm wide with a length the same as the width of the wallcovering. Repeat this
30、 at approximately 1 m intervals throughout the length of the roll. Cut the strips into rectangles (50 1) mm long3 (30 1) mm wide (see figure 1). 4.4.1.2 Borders Cut a strip of (30 1) mm width through the whole length of the border. Cut this strip into rectangles of (50 1) mm length. Use the appropri
31、ate number of rolls to produce at least 50 rectangles (see figure 2). 4.4.2 Selection of test specimens Select by visual inspection the 10 rectangles which have the maximum amount of coating and/or the deepest yellow or red colour. Condition in accordance with ISO 187. Cut these 10 rectangles into s
32、quares of approximately 6m m36 mm and mix the squares obtained. 4.5 Procedure 4.5.1 Extraction method Weigh to the nearest milligram (1 0,05) g of the small squares (4.4.2) in a glass container of approximately 100 ml capacity. Add (50 0,1) ml of the hydrochloric acid (4.2.2) at (37 2) C. Shake vigo
33、rously for 1 min, determine the pH of the solution (4.3.2). If the pH is higher than 1,5 add dropwise, while shaking, the hydrochloric acid (4.2.3) until the pH is below 1,5 and above 1,0. Mount the container on a shaker (4.3.3) and place in the oven (4.3.4) at (37 2) C, shake the mixture at (37 2)
34、C for (60 2) min, then allow to stand at (37 2) C for (60 2) min. Filter immediately through the 0,45mm pore size filter (4.3.5) and collect the filtrate for the determination of the heavy metal (or other elements) content.Page 4 EN 12149 : 1997 BSI 1998 1 2 1 m 30 mm 30 mm 50 mm 3 1. Roll width 2.
35、Strip 3. Rectangles Figure 1. 1 30 mm 1. Rectangles 50 mm Figure 2.Page 5 EN 12149 : 1997 BSI 1998 4.5.2 Determination of extracted heavy metals (and other elements) Use a method having a detection limit not exceeding 1/10 of the specified limit values. NOTE 1. The detection limit is estimated at th
36、ree times the standard deviation of the blank test value of the method being used. NOTE 2. In principle, the methods given below (non-exhaustive list) satisfy the above condition: atomic absorption spectrometry; ICP emission spectrometry. 4.6 Expression of results Calculate the heavy metal extracted
37、 for each metal (or element) in milligrams per kilogram of wallcovering from the following equation: R = 3 50 (1) c m where R is the determined heavy metal (or element) content, in milligrams per kilogram of wallcovering; c is the concentration of the heavy metal (or element) in the extract, as dete
38、rmined by the method of 4.5.2, in milligrams per litre; m is the test portion, in grams. 5 Test B: Determination of vinyl chloride monomer 5.1 Principle Dissolution or suspension of a test portion in a suitable solvent and determination of the vinyl chloride content by gas chromatography using the h
39、ead-space method. 5.2 Reagents 5.2.1 During the analysis, unless otherwise stated, use only reagents of recognized analytical grade suitable for gas chromatography and water of equivalent purity to grade 3 of EN ISO 3696. 5.2.2 Vinyl chloride (pure): lecture bottle fitted with fine adjustment valve.
40、 5.2.3 N,N-dimethyl acetamide. 5.2.4 Hydrogen. 5.2.5 Nitrogen. 5.2.6 Air. 5.3 Standard solutions 5.3.1 Preparation of stock solution Take 50 ml of N,N-dimethyl acetamide (5.2.3) and weigh. Bubble vinyl chloride through for approximately 10 s, until a concentration of approximately 10 g/l is obtained
41、, re-weigh and seal the container. 5.3.2 Diluted standard Take the solution prepared in accordance with 5.3.1 and further dilute by a factor of 500 (20 mg/l). For example, dilute 10ml of stock to 5 ml with the N,N-dimethyl acetamide. 5.4 Test apparatus 5.4.1 Usual laboratory apparatus. 5.4.2 Gas chr
42、omatograph, fitted with an automatic headspace sampler, or with facilities for manual sample injection, and a flame ionization detector. 5.4.3 Gas chromatographic column, capable of completely separating the air peak, and the vinyl chloride peak from the standard solution (5.3.2) and the internal st
43、andard peak, if used. The signal obtained from the column in use with a solution containing 0,02 mg of vinyl chloride per litre or kilogram shall be at least five times that of the background noise. 5.5 Test specimens 5.5.1 Preparation of test specimens 5.5.1.1 Roll (except borders) Take a roll of w
44、allcovering and make two cuts across the width of the wallcovering to produce a strip (30 1) mm wide with a length the same as the width of the wallcovering. Repeat this at approximately 1 m intervals throughout the length of the roll. Cut the strips into rectangles (50 1) mm long3 (30 1) mm wide (s
45、ee figure 3). 5.5.1.2 Borders Cut a strip of (30 1) mm width through the whole length of the border. Cut this strip into rectangles of (50 1) mm length. Use the appropriate number of rolls to produce at least 50 rectangles (see figure 4). 5.5.2 Selection of test specimens Select by visual inspection
46、 the 10 rectangles most representative of the overall decoration. Condition in accordance with ISO 187. Cut these 10 rectangles into squares of approximately 6m m36 mm and mix the squares obtained. 5.6 Procedure 5.6.1 Preparation of test solutions Weigh accurately 0,5 g of the test specimens (5.5.2)
47、 into a headspace vial of 10 ml maximum capacity and add 2 ml of N,N-dimethyl acetamide (5.2.3). Close the vial. 5.6.2 Preparation of the calibration solution Into each of five vials, introduce 2 ml of N,N-dimethyl acetamide (5.2.3) and add to each the appropriate volume of the diluted standard solu
48、tion such that a series of solutions is obtained approximately 0 ng, 125 ng, 250 ng, 375 ng and 500 ng of vinyl chloride monomer. Close the vials.Page 6 EN 12149 : 1997 BSI 1998 1 1 m 30 mm 1. Roll width 2. Strip 3. Rectangles 2 30 mm 50 mm 3 Figure 3. 1 30 mm 1. Rectangles 50 mm Figure 4.Page 7 EN
49、12149 : 1997 BSI 1998 5.6.3 Procedure for gas chromatography 5.6.3.1 Place the vials containing the test solutions (5.6.1) and the calibration solutions (5.6.2)i n a water bath controlled at (60 1) C for 2 h to attain equilibrium. Agitate the vials, avoiding contact between the liquid and stopper, to obtain, in the vials containing the test
