1、BRITISH STANDARDBS EN 71-11:2005Safety of toys Part 11: Organic chemical compounds Methods of analysisThe European Standard EN 71-11:2005 has the status of a British StandardICS 97.200.50g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g
2、55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 71-11:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 22 November 2005 BSI 22 November 2005ISBN 0 580 46391 5National forewordThis British Standa
3、rd is the official English language version of EN 71-11:2005. The UK participation in its preparation was entrusted to Technical Committee CW/15, Safety of toys, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enq
4、uiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.A list of organizations represented on this committee can be obtained on request to its secretary.Cross-referencesThe British S
5、tandards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.T
6、his publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard does not of itself confer immunity from legal obligations.Summary of pagesThis document comprises a front cover, an inside fron
7、t cover, the EN title page, pages 2 to 69 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 71-11November 2005ICS 97.200.50English
8、 VersionSafety of toys - Part 11: Organic chemical compounds - Methodsof analysisScurit des jouets - Partie 11 : Composs chimiquesorganiques dans les jouets - Mthodes danalyseSicherheit von Spielzeug - Teil 11: Organisch-chemischeVerbindungen - AnalysenverfahrenThis European Standard was approved by
9、 CEN on 27 June 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards m
10、ay 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 translationunder the responsibility of a CEN member into its own language and notified to the Cent
11、ral Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Polan
12、d, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means rese
13、rvedworldwide for CEN national Members.Ref. No. EN 71-11:2005: EEN 71-11:2005 (E) 2 Contents Page Foreword 3 Introduction4 1 Scope .5 2 Normative references .5 3 Terms and definitions.5 4 Environmental, health and safety precautions .6 5 Methods of analysis6 5.1 General 6 5.2 Flame retardants .6 5.3
14、 Colourants.9 5.4 Primary aromatic amines15 5.5 Monomers and solvents .19 5.6 Wood preservatives37 5.7 Preservatives.41 5.8 Plasticisers44 Annex A (informative) Methods of analysis for volatile solvents .48 Annex B (informative) Validation of test methods .65 Annex C (informative) Colourants conform
15、ational analysis 66 Annex ZA (informative) Clauses of this European Standard addressing essential requirements or other provisions of EU Directives68 Bibliography.69 EN 71-11:2005 (E) 3 Foreword This European Standard (EN 71-11:2005) has been prepared by Technical Committee CEN/TC 52 “Safety of Toys
16、”, the secretariat of which is held by DS. 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 2006, and conflicting national standards shall be withdrawn at the latest by May 2006. This European
17、Standard has been prepared under a mandate given to CEN by the European Commission and the European Free Trade Association, and supports essential requirements of EU Directive(s). For relationship with EU Directive(s), see informative Annex ZA, which is an integral part of this European Standard. Th
18、is European Standard constitutes part 11 of the European Standard on Safety of Toys. This part should be read in conjunction with parts 9 and 10. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European St
19、andard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 71-11:2005 (E) 4
20、Introduction The European Standard EN 71 for “safety of toys” consists of the following parts: Part 1: Mechanical and physical properties Part 2: Flammability Part 3: Migration of certain elements Part 4: Experimental sets for chemistry and related activities Part 5: Chemical toys (sets) other than
21、experimental sets Part 6: Graphical symbols for age warning labelling Part 7: Finger paints Requirements and test methods Part 8: Swings, slides and similar activity toys for indoor and outdoor family domestic use Part 9: Organic chemical compounds Requirements Part 10: Organic chemical compounds Sa
22、mple preparation and extraction Part 11: Organic chemical compounds Methods of analysis The European Standards EN 71-9, EN 71-10 and EN 71-11 were mandated by the European Commission (M/229) to address the risks presented by organic chemical compounds in toys by taking into account the potential exp
23、osure and toxicological effects of those substances considered to present the greatest risk to health. This European Standard specifies methods of analysis to enable assessment of compliance with the chemical requirements specified in EN 71-9 when toy and toy material extracts have been prepared acc
24、ording to the sampling procedures in EN 71-10. This part on methods of analysis should be read in conjunction with EN 71-9, which contains requirements for certain organic chemical compounds in toys, and EN 71-10, which describes sample preparation and extraction procedures. This European Standard t
25、akes into account the opinion of the Toxicology Section of the Scientific Advisory Committee published in 1992 (EUR 13976), which recommended that certain groups of chemical compounds used in toys and toy materials need to be given special attention. In drafting this European Standard CEN/TC 52 has
26、considered organic chemicals that can be classified within the following groups: Solvents Preservatives Plasticisers (excluding phthalate plasticisers)1 Flame retardants Monomers Biocides (wood preservatives) Processing aids Colouring agents 1Phthalate plasticisers were specifically excluded from th
27、e scope of mandate M/229. EN 71-11:2005 (E) 5 1 Scope This Part 11 of the European Standard EN 71 for safety of toys specifies methods for the analysis of toy and toy material extracts prepared according to the sampling procedures in EN 71-10, to enable assessment of compliance with the chemical req
28、uirements specified in EN 71-9. This European Standard specifies analytical methods for the identification and determination of the following groups of organic chemicals: Flame retardants Colourants Primary aromatic amines Monomers and solvents Wood preservatives Preservatives Plasticisers NOTE 1 Me
29、thods for formaldehyde in accessible textile components of toys; accessible paper components of toys; and accessible resin-bonded wood components of toys are specified in EN 71-9. NOTE 2 The method for free formaldehyde as a preservative is specified in EN 71-10. 2 Normative references The following
30、 referenced documents are indispensable for the application of this European Standard. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 71-9:2005, Safety of toys Part 9: Organic chemical
31、 compounds Requirements EN 71-10:2005, Safety of toys Part 10: Organic chemical compounds Sample preparation and extraction EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) 3 Terms and definitions For the purposes of this European Standard, the followin
32、g terms and definitions apply. 3.1 action limit routinely-achievable limit of quantification for a particular substance using the specified method of analysis 3.2 aqueous migrate liquid obtained after extracting a toy material according to the procedure specified in Clause 6 of EN 71-10:2005 3.3 tes
33、t portion portion of the laboratory sample prepared for analysis 3.4 toy material material from which toys and toy components are made NOTE This definition differs from that given in EN 71-3 EN 71-11:2005 (E) 6 4 Environmental, health and safety precautions When preparing this European Standard, con
34、sideration was given to the minimisation of environmental impacts caused by the use of the methods of analysis. It is the users responsibility to use safe and proper techniques in handling materials in the methods of analysis specified in this European Standard. Consult manufacturers for specific de
35、tails such as material safety data sheets and other recommendations. Wear protective goggles and coats in all laboratory areas. Be careful about substances, which are toxic and/or human carcinogens. A fume cupboard shall be used during preparation of organic solvent solutions. Solvents shall be disp
36、osed of in accordance with environmental requirements. 5 Methods of analysis 5.1 General All chemicals used for analysis shall be of analytical grade (pro analysis) or, if unavailable, the best technical grade. Water shall be of grade 3 according to EN ISO 3696 or of a comparable quality, and demons
37、trably free from analytes of interest. The precision of volumetric glassware should be grade A. The analysis of toys and toy materials for chemical compounds for which limits are given in Tables 2 A to 2 I of EN 71-9:2005 shall be performed in accordance with the sampling procedures specified in EN
38、71-10 and the methods of analysis described in this European Standard. Alternative methods of analysis are acceptable only if they are capable of achieving at least the accuracy and precision of the methods described in this European Standard; an adequate sensitivity; and have been validated to show
39、 that the results are equivalent to those of these standard methods. 5.2 Flame retardants NOTE Methods are given for pentabromodiphenyl ether and octabromodiphenyl ether in order to enable compliance with Directive 2003/11/EC of the European Parliament and of the Council to be demonstrated for texti
40、le toy materials. 5.2.1 Principle Flame retardants are determined in acetonitrile extracts of toy materials by liquid chromatography with diode-array and mass spectrometry detection (LC-DAD-MS) using the external standard method of calibration. EN 71-11:2005 (E) 7 5.2.2 Standards, reagents and solve
41、nts 5.2.2.1 Standards 5.2.2.1.1 Pentabromodiphenyl ether2*, CAS No. 32534-81-9 5.2.2.1.2 Octabromodiphenyl ether3* , CAS No. 32536-52-0 5.2.2.1.3 Tri-o-cresyl phosphate, CAS No. 78-30-8 5.2.2.1.4 Tris(2-chloroethyl) phosphate, CAS No. 115-96-8 5.2.2.2 Reagents and solvents 5.2.2.2.1 Acetonitrile 5.2
42、.2.2.2 Dichloromethane 5.2.2.2.3 Ammonium acetate, anhydrous 5.2.2.2.4 Acetic acid, glacial 5.2.2.2.5 Ammonium acetate, 10 mmol/l aqueous solution, pH 3,6 Transfer (0,77 0,01) g ammonium acetate (5.2.2.2.3) into a 1 000-ml volumetric flask, add 980 ml of water, adjust the pH to 3,6 0,1 with glacial
43、acetic acid and make up to the mark with water. 5.2.2.3 Stock standard solution (100 mg/l) Weigh, to the nearest 0,1 mg, (10 1) mg of each flame retardant (5.2.2.1) into a 100-ml volumetric flask. Add 25 ml of acetonitrile (5.2.2.2.1) and mix carefully to dissolve. Place in an ultrasonic bath for 10
44、 min to ensure complete dissolution. Make up to the mark with acetonitrile. The stability of the mixed stock standard solution should be checked regularly. It should be stable for up to 6 months when stored in the dark at (4 2) C. 5.2.3 Apparatus Liquid chromatograph with diode-array and mass spectr
45、ometer detectors The following LC-DAD-MS conditions for flame retardant determination have been found to be suitable: Column: C18, 80 , 3,5 m, double endcapped, (Zorbax Eclipse XDB4, or equivalent) 2,1 mm x 150 mm Guard column: C18, 80 , 4 mm x 2,0 mm, Mobile phase A: Ammonium acetate solution, 10 m
46、mol/l, pH 3,6 (5.2.2.2.5) Mobile phase B: Acetonitrile Gradient: see Table 1 2This substance is also known as pentabromodiphenyl oxide. *There are no requirements in EN 71-9 for this substance. 3This substance is also known as octabromodiphenyl oxide. 4Zorbax Eclipse XDB is an example of a suitable
47、product available commercially. This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of this product. EN 71-11:2005 (E) 8 Injection volume: 5 l Run time: 45 min Flow: 0,3 ml/min DAD mode: 240 nm 20 nm DAD range: 200 nm to 800
48、nm Nebulizer: 200 Kpa Dry gas: 10 l/min MS range: 110 m/z to 500 m/z MS mode: Scan positive Ionisation: ESI+ Fragmentor: 80 V Table 1 Gradient program Time min Mobile phase A % Mobile phase B % 0 60 407 40 60 17 2 9835 2 98 45 60 405.2.4 Procedure 5.2.4.1 Calibration solutions Prepare a series of mi
49、xed flame retardant calibration solutions from the stock standard solution (5.2.2.3) at 1,0 mg/l, 2,0 mg/l, 4,0 mg/l and 8,0 mg/l concentrations in acetonitrile. 5.2.4.2 Determination Proceed to liquid chromatographic determination using the conditions described in 5.2.3. Inject the calibration solutions (5.2.4.1) and the extract obtained at 8.1.1 of EN 71-10:2005. 5.2.4.3 Identification For a positive identification, the peak purity factor should achieve a match of at least 85 %. 5.2.5
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