1、 STDoBSI BS EN IS0 3451-4-ENGL 2000 m Lb24bb 0660025 9T7 BRITISH STANDARD Plastics - Determination of ash - Part 4: Polyamides The European Standard EN IS0 345142000 has the status of a British Standard ICs 83.080.20 BS EN IS0 3451-4:ZOOO NO COPYING WITHOUT BSI PERMISSION EXCEPT As PERMIITED BY COPY
2、RIGHT LAW STD.BS1 BS EN IS0 3451-4-ENGL 2000 P Lb24bh OB8OOZb 835 W BS EN IS0 3451-4:2000 direction of the Sector Committee for Materiais and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 November 2000 Amd. No. O BSI 11-2000 National foreword Dat
3、e Comments This British Standard is the officiai English language version of EN IS0 34514:2000. It is identical with IS0 345141998. It supersedes BS EN IS0 34514:1996 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics, which h
4、as the responsibility to: - aid enquirers to understand the text; - present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed - monitor related intemational and European developments and promulgate the
5、m in the UK A list of organizations represented on tkis committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their correspond
6、ing European publications. The British Standards which implement 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 Standa
7、rds Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of page
8、s This document comprises a front cover, an inside front cover, the EN IS0 title page, the EN IS0 foreword page, the IS0 title page, pages ii and iii, a blank page, pages 1 to 5, the annex ZA page, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates w
9、hen the document was last issued. ISBN O 580 36678 2 STD-BSI BS EN IS0 3451-4-ENGL 2000 = 1b24bb9 0880027 771 = EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN IS0 3451-4 September 2000 ICs 83.080.20 Supersedes EN IS0 3451-4:1995 English version Plastics - Determination of ash - Part 4: Polyami
10、des (IS0 3451- 4: 1 998) Plastiques - Dtermination du taux de cendres - Partie 4: Polyamides (IS0 3451-4:1998) Kunststoffe - Bestimmung der Asche - Teil 4: Polyamide (IS0 3451-41998) This European Standard was approved by CEN on 8 September 2000. CEN members are bound to comply with the CENKENELEC I
11、ntemal 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 mem
12、ber. 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 member
13、s 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 United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMITE EUROPEEN DE NORMALISATI
14、ON EUROPISCHES KOMITEE FR NORMUNG Central Secretariat: rue de Stassart, 36 6-1050 Brussels O 2000 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN IS0 3451-4:2000 E STD.BSI BS EN IS0 3451-4-ENGL 2000 Lb24bb9 0880028 608 EN IS0 3451-
15、4:ZOOO Foreword The text of the International Standard from Technical Committee ISOlTC 61 “Plastics“ of the International Organization for Standardization (ISO) has been taken over as an European Standard by Technical Committee CENlTC 249 “Plastics“, the secretariat of which is held by IBN. This Eur
16、opean Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by March 2001, and conflicting national standards shall be withdrawn at the latest by March 2001. This European Standard supersedes EN IS0 3451 -4:1995. Accord
17、ing to the CENKENELEC 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, Italy, Luxembourg, Netherlands, Norway, Portugal,
18、Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard IS0 3451 -4:1998 has been approved by CEN as a European Standard without any modification. NOTE: Normative references to International Standards are listed in annex ZA (normative). STD*BSI BS
19、 EN IS0 3451-4-ENGL 2000 II 1b24hbq cB80029 544 EN IS0 3451-4:2000 INTERNATIONAL STANDARD IS0 3451 -4 Second edition 1998-1 2-1 5 Plastics - Determination of ash - Part 4: Polyamides Plastiques - Dtermination du taux de cendres - Pattie 4: Polyamides Reference number IS0 3451-4:1998(E) STD.BSI BS EN
20、 IS0 3451-4-ENGL 2000 118 Lh24hh 0880030 266 EN IS0 3451-49000 Contents 1 Scope 1 2 Normative reference 1 3 Principle 1 3.1 Unfilled materials 1 3.2 Filled and glass-fibre reinforced materials 1 3.3 Flame-retardant materials reinforced with glass fibre 2 4 Reagents (method C or method A in the prese
21、nce of DBB) . 2 5 Apparatus . 2 6 Procedure . 2 6.1 Test portion . 2 6.2 Unfilled materials 3 6.3 Filled and glass-fibre reinforced materials 3 6.4 Materials reinforced with glass fibre containing flame-retardant antimony trioxide and/or other volatilizable additives . 3 7 Expression of results 4 8
22、Precision . 4 9 Test report 4 II STD.BS1 BS EN IS0 3453-4-ENGL 2000 Zb24bb 0880033 LT2 = EN IS0 3451-42000 Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards bodies (IS0 member bodies). The work of preparing International Standards is no
23、rmally carried out through IS0 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 part in
24、 the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draf International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard r
25、equires approval by at least 75 % of the member bodies casting a vote. International Standard IS0 3451 -4 was prepared by Technical Committee ISOTTC 61, Plastics, Subcommittee SG 5, Physical-chemical properties. This second edition cancels and replaces the first edition (IS0 3451 -4:1986), which has
26、 been technically revised. IS0 3451 consists of the following parts, under the general title Plastics - Determination of ash: - Part 1: General methods - Part 2: Poly(alky1ene terephthalate) materials - Part 3: Unplasticized cellulose acetate - Part 4: Polyamides - Part 5: Poly(viny1 chloride) . 111
27、 STD-BSI BS EN IS0 3q51-4-ENGL 2000 W lb24bb7 0880032 O37 EN IS0 3451-4:2000 Plastics - Determination of ash - Part 4: Pol yam ides WARNING - This part of IS0 3451 may involve hazardous chemicals, materials and operations. This part of IS0 3451 does not purport to address the safety problems associa
28、ted with its use. It is the responsibility of the user to establish proper safety and health practices and determine the applicability of regulatory limitations prior to use. 1 Scope This part of IS0 3451 specifies methods for determination of the ash of polyamides, both filled and unfilled. The gen
29、eral procedures given in IS0 3451-1 are followed. For unfilled materials method A or method C of IS0 3451-1:1997 is used. For filled and glass-fibre reinforced materials method A of IS0 3451-1:1997 is used. For glass-fibre filled materials containing flame retardant, antimony trioxide, and/or other,
30、 volatilizable, additives such as pigment zinc sulfide, a modification is incorporated to remove these as volatile bromine component(s). 2 Normative reference The following standard contains provisions which, through reference in this text, constitute provisions of this patt of IS0 3451. At the time
31、 of publication, the edition indicated was valid. All standards are subject to revision, and parties to agreements based on this part of IS0 3451 are encouraged to investigate the possibility of applying the most recent edition of the standard indicated below. Members of IEC and IS0 maintain registe
32、rs of currently valid International Standards. IS0 3451 -1 :1997, Plastics - Determination of ash - Part 1: General methods. 3 Principle 3.1 Unfilled materials Direct calcination by burning the organic matter and treating the residue at a high temperature until constant mass is reached (IS0 3451 -1
33、:I 997, method A). If the material contains metal halides and/or metals (especially in the presence of halogenated material) which are liable to evaporate during burning of the organic matter, calcination after sulfation can be applied (IS0 3451-1:1997, method C). This procedure is carried out by he
34、ating the organic matter together with concentrated sulfuric acid up to a temperature where fuming and subsequent burning of the organic matter occurs, and finally treating the residue at a high temperature until constant mass is reached. 3.2 Filled and glass-fibre reinforced materials Direct calcin
35、ation, by burning the organic matter and treating the residue at a high temperature until constant mass is reached (IS0 3451 -1 :1997, method A) (see note 1 in 3.3). 1 3.3 Flame-retardant materials reinforced with glass fibre Calcination by burning the organic matter in the presence of decabromobiph
36、enyl (DBB) and finally treating the residue at a high temperature until constant mass is reached (IS0 3451-1:1997, method A). NOTE 1 Some additives, for instance zinc sulfide, are also completely volatilized as bromides by burning the organic matter in contact with decabromobiphenyl (DBB). Informati
37、on with respect to the additive(s) present in the material and the potential to evaporate during burning in contact with DBB should be requested from the supplier or obtained by testing on the pure chemical. NOTE 2 Flame retardants with a high bromine content, for instance ethylene bis(tetrabromopht
38、ha1imide) or brominated polystyrene may also be used. The applicability and amount of chemical to be used can be determined by carrying out ash determinations in accordance with 6.4 with increasing amounts of flame retardant until a constant result is obtained. The chemical should be applied as a po
39、wder. 4 Reagents (method C or method A in the presence of DBB) During the analysis, use only reagents of analytical grade or specified grade and only distilled water or water of equivalent purity. 4.1 Ammonium carbonate, anhydrous. 4.2 Ammonium nitrate, approximately 1 O % (mh) solution. 4.3 Sulfuri
40、c acid, p 1,84 g/ml. 4.4 Decabromobiphenyl (DBB), powder, technical grade or higher purity. WARNING - The use of decabromobiphenyl may result in the formation of dioxins. Temperatures in the order of 600 OC to 850 OC are generally known as ideal temperatures for the formation of dioxins. 5 Apparatus
41、 Apparatus specified in clause 4 of IS0 3451 -1 :1997, and in particular: 5.1 Crucibles of silica, porcelain or platinum, inert to the material tested, and typically of diameter (upper part) 50 mm to 60 mm and height equal to the diameter (see note 2 in 3.3). 5.2 Muffle furnace, capable of being mai
42、ntained at (600 k 25) OC, (850 k 50) “C or at a minimum temperature of 850 “C. 5.3 Fume cupboard. 6 Procedure The material shall be in the form of small pieces of 1 cm x 0,5 cm x 0,2 cm or smaller, granules or powder. Filled or reinforced materials shall be dried before calcination, .e. by heating a
43、t 1 O0 “C until constant mass is reached. 6.1 Test portion Take a quantity of the test sample sufficient to yield 5 mg to 200 mg of ash (see table 1). In the case of reinforced materials, take a test portion of 2 g or more. If the likely quantity of ash is unknown, carry out a preliminary ash determ
44、ination. According to the approximate ash content, choose the size of the test portion to be used from table 1. 2 STD-BSI BS EN IS0 345L-4-ENGL 2000 Lb24bb9 0880034 901 EN IS0 3451-4:2000 Table 1 - Mass of test portion 6.2 Unfilled materials Follow the procedure described in IS0 3451-1:1997, method
45、A, applying a calcination temperature of (850 k 50) OC. If the material contains metal halides or metals in the presence of halogenated material, liable to evaporate during the calcination procedure, or in those cases where “sulfated ash“ is required, method C shall be applied (IS0 3451-1:1997, meth
46、od C). 6.3 Filled and glass-fibre reinforced materials Follow the procedure described in IS0 3451 -1 :1997, method A, applying a calcination temperature of (850 f 50) “C. If at that temperature glass fibres present become molten and thus prevent further calcination of the polymer, lower the temperat
47、ure of calcination to (600 * 25) “C and repeat the procedure with a fresh test portion. 6.4 Materials reinforced with glass fibre containing flame-retardant antimony trioxide and/or other volatilizable additives The sample shall be ground or cut to pieces of 1 cm x 0,5 cm x 0,2 cm or smaller. Procee
48、d as in 5.3.1 and 5.3.2 of IS0 3451-1 :1997, method A. Add to the sample a quantity of DBB (4.4) equal to half the mass of the sample in grams and mix well in the crucible. Place the crucible in the muffle furnace, applying a calcination temperature of at least 850 OC. The muffle furnace shall be pl
49、aced in a fume cupboard. Continue as directed in IS0 3451-1:1997, from 5.3.4 of method A. , Directly placing the crucible into the muffle furnace is preferred. If direct calcination leads to large differences between repeated tests, for instance due to loss of ash-containing material, gently heat the crucible over a quiet flame until formation of fumes ceases. Make sure that the volatile components are properly drawn off by a fume cupboard. Place the crucible in the muffle furnace and apply a calcination temperature of at least 850 OC. Continue as directed in
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