1、BRITISH STANDARDBS EN ISO 11402:2005Incorporating Corrigendum No. 1Phenolic, amino and condensation resins Determination of free-formaldehyde contentThe European Standard EN ISO 11402:2005 has the status of a British StandardICS 83.080.10g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g4
2、4g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 11402:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 24 March 2005 BSI 2006ISBN 0 580 456
3、32 3 National forewordThis British Standard is the official English language version of EN ISO 11402:2005 including Corrigendum May 2006. It is identical with ISO 11402:2004. It supersedes BS EN ISO 11402:1998, BS EN ISO 9397:1997 and BS EN ISO 9020:1998 which are withdrawn.The UK participation in i
4、ts preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting plastics and prepegs, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement in
5、ternational 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.This publication does not pu
6、rport 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. aid enquirers to understand the text; present to the responsible international/European committ
7、ee 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.Summary of pagesThis document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO f
8、oreword page, the ISO title page, pages ii to iv, pages 1 to 12, an inside back cover 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 Comments16475 30 June 2006 Correction of supersessio
9、n detailsEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 11402 February 2005 ICS 83.080.10 Supersedes EN ISO 11402:1998, EN ISO 9397:1997 and EN ISO 9020:1998 English version Phenolic, amino and condensation resins - Determination of free-formaldehyde content (ISO 11402:2004) Rsines phnoliq
10、ues, aminiques et de condensation - Dosage du formaldhyde libre (ISO 11402:2004) Phenol-, Amin- und Kondensationsharze - Bestimmung des Gehalts an freiem Formaldehyd (ISO 11402:2004) This European Standard was approved by CEN on 3 February 2005. CEN members are bound to comply with the CEN/CENELEC I
11、nternal 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 standards may be obtained on application to the Central Secretariat or to any CEN me
12、mber. 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 the Central Secretariat has the same status as the official versions. CEN membe
13、rs 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, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and Unit
14、ed Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 11402:
15、2005: EForeword The text of ISO 11402:2004 has been prepared by Technical Committee ISO/TC 61 “Plastics” of the International Organization for Standardization (ISO) and has been taken over as EN ISO 11402:2005 by Technical Committee CEN/TC 249 “Plastics“, the secretariat of which is held by IBN. Thi
16、s 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 August 2005, and conflicting national standards shall be withdrawn at the latest by August 2005. This document supersedes EN ISO 11402:1998, EN ISO 939
17、7:1997 and EN ISO 9020:1998. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Icelan
18、d, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 11402:2004 has been approved by CEN as EN ISO 11402:2005 without any modifications. EN ISO 11402:2005R
19、eference numberISO 11402:2004(E)OSI 4002INTERNATIONAL STANDARD ISO11402Second edition2004-03-15Phenolic, amino and condensation resins Determination of free-formaldehyde content Rsines phnoliques, aminiques et de condensation Dosage du formaldhyde libre EN ISO 11402:2005IS:20411 O4002(E) DPlcsid Fre
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24、euqer ehe.r ISO cirypothg fofice saCe tsopale 65 eneG 1121-HC 02 avleT. 4 + 10 947 22 1 11 xaF0 947 22 14 + 9 74 E-mail coirypthgiso.o grWe bwww.is.o groPulbisdehi n Switlrez dnaii ISO 4002 Allr ithgsr esedevrIS:20411 O4002(E) I SO 4002 All irthgs ersedevr iiiContents Page Foreword iv 1 Scope1 2 Nor
25、mative references1 3 Terms and definitions .2 4 Test procedures 2 4.1 General .2 4.2 Hydroxylamine hydrochloride procedure.2 4.3 Sulfite procedure.4 4.4 KCN procedure 7 5 Test report10 Annex A (informative) Suitability of the procedures for different types of resin.11 Annex B (informative) Removal o
26、f Hg2+and CNfrom mercury and cyanide residues12 EN ISO 11402:2005IS:20411 O4002(E) iv I SO 4002 All irthgs ersedevrForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standar
27、ds is normally carried out through ISO technical committees. Each member body interested in a subject for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take
28、 part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is
29、to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility
30、 that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 11402 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials. This second edition cancel
31、s and replaces the first edition (ISO 11402:1993), as well as ISO 9020:1994 and ISO 9397:1995. The three standards have been combined into one, the sulfite procedure being taken from ISO 9020 and the hydroxylamine hydrochloride procedure from ISO 9397. EN ISO 11402:2005INTENRATIONAL TSANDADR IS:2041
32、1 O4002(E)I SO 4002 All irthgs ersedevr 1Phenolic, amino and condensation resins Determination of free-formaldehyde content 1 Scope This International Standard specifies three methods for determining the free-formaldehyde content in the following: a) Phenolic resins, by potentiometric titration in a
33、queous or organic solution (hydroxylamine hydrochloride procedure). The method is applicable to resins with free-formaldehyde contents up to and including 15 % by mass. For free-formaldehyde contents between 15 % by mass and 30 % by mass, it may be necessary to adjust the concentrations of the stand
34、ard volumetric solutions used accordingly. b) Amino resins and furan resins (sulfite procedure). The method is applicable to resins resulting from the polycondensation of urea and melamine with formaldehyde and to furan resins resulting from the polycondensation of furfuryl alcohol with formaldehyde
35、 without further modification. c) Condensation resins (KCN procedure), including urea resins, furan resins, melamine resins and phenolic resins, as well as combinations and modifications of these resins. The purpose of this International Standard is to establish recognized and useful determination p
36、rocedures (for instance in order to check whether official regulations on the handling of hazardous workplace materials are observed). As far as possible, all formaldehyde-containing resins are to be included in this connection. The free-formaldehyde content determined in formaldehyde condensation r
37、esins using this International Standard represents the actual content at the time of the determination. The value bears no quantitative relationship to the free-formaldehyde content during or after processing. 2 Normative references The following referenced documents are indispensable for the applic
38、ation of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 385-1, Laboratory glassware Burettes Part 1: General requirements ISO 648, Laboratory glassware One-mark pipette
39、s ISO 3696, Water for analytical laboratory use Specification and test methods ISO 15528, Paints, varnishes and raw materials for paints and varnishes Sampling EN ISO 11402:2005IS:20411 O4002(E) 2 I SO 4002 All irthgs ersedevr3 Terms and definitions For the purposes of this document, the following t
40、erms and definitions apply. 3.1 free formaldehyde formaldehyde that is present in unbound form as formaldehyde, formaldehyde dihydrate (dihydroxymethylene) or polyoxymethylene in a condensation resin 4 Test procedures 4.1 General The choice of test procedure for the determination of free formaldehyd
41、e in condensation resins is made in accordance with Table 1. Table 1 Selection of procedure Procedure Suitable for testing of Hydroxylamine hydrochloride procedure Phenolic resins, furan resinsa(unmodified with urea or melamine resin) Sulfite procedure Urea resins, melamine resins, furan resinsa, ur
42、ea-melamine resins, furan-urea resins KCN procedurebMelamine-phenolic resins, urea-phenolic resins, urea-melamine-phenolic resins aSee Annex A, Clause A.2. bSee Annex A, Clause A.3. 4.2 Hydroxylamine hydrochloride procedure 4.2.1 Principle The formaldehyde is converted to the oxime with hydroxylamin
43、e hydrochloride. The hydrochloric acid formed during this reaction is determined by potentiometric back-titration, using sodium hydroxide solution. Oximation reaction: CH2O + NH2OHHCl CH2NOH + HCl + H2O 4.2.2 Reagents During the analysis, use only reagents of recognized analytical grade and only wat
44、er of at least grade 3 purity as defined in ISO 3696. 4.2.2.1 Hydroxylamine hydrochloride, 10 % by mass solution, the pH of which has been adjusted to 3,5 by the addition of sodium hydroxide solution. 4.2.2.2 Sodium hydroxide, standard volumetric solutions, c(NaOH) = 1 mol/l and c(NaOH) = 0,1 mol/l.
45、 4.2.2.3 Hydrochloric acid, standard volumetric solutions, c(HCl) = 1 mol/l and c(HCl) = 0,1 mol/l. 4.2.2.4 Methanol, free of aldehydes and ketones. EN ISO 11402:2005IS:20411 O4002(E) I SO 4002 All irthgs ersedevr 34.2.2.5 Propan-2-ol, free of aldehydes and ketones. 4.2.3 Apparatus Ordinary laborato
46、ry apparatus and glassware, together with the following: 4.2.3.1 Balance, accurate to 0,1 mg. 4.2.3.2 pH-meter, sensitive to 0,1 pH-units, equipped with a glass indicating electrode and a standard calomel reference electrode. 4.2.3.3 Magnetic stirrer. 4.2.3.4 Graduated burettes, of capacity 10 ml an
47、d 25 ml, the latter being for use if the formaldehyde content is likely to be greater than 5 % by mass. 4.2.4 Sampling Take a representative sample of the product to be tested, as described in ISO 15528. 4.2.5 Procedure 4.2.5.1 Test temperature Carry out the test at (23 1) C. 4.2.5.2 Test portion We
48、igh, to the nearest 0,1 mg, into a 250 ml beaker, a test portion of mass from 1 g to 5 g, depending on the assumed formaldehyde content (see Table 2). Table 2 Mass of test portion Assumed formaldehyde content% by mass Mass of test portion g 4 1 to 2 4.2.5.3 Determination Add 50 ml of methanol (4.2.2
49、.4), or 50 ml of a mixture of 3 volumes of propan-2-ol (4.2.2.5) and 1 volume of water, to the contents of the beaker, switch on the magnetic stirrer (4.2.3.3) and stir until the resin has dissolved and the temperature has stabilized at (23 1) C. Introduce the electrodes of the pH-meter (4.2.3.2) into the solution and, using the 0,1 mol/l solution of hydrochloric acid (for neutralized resins) or the 1 mol/l solution (for highly alkaline resins) (see 4.2.2.3), adjust the pH to 3,5. Pipette into the solution approximat
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