1、BS EN ISO3451-1:2008ICS 83.080.01NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDPlastics Determination of ashPart 1: General methods (ISO3451-1:2008)This British Standard was published under theauthority of the StandardsPolicy and StrategyCommittee on 32008 BSI
2、 2008ISBN 978 0 580 57206 7Amendments/corrigenda issued since publicationDate CommentsBS EN ISO 3451-1:2008National forewordThis British Standard is the UK implementation of EN ISO 3451-1:2008.It supersedes BS EN ISO 3451-1:1997 which is withdrawn.The UK participation in its preparation was entruste
3、d to TechnicalCommittee PRI/21, Testing of plastics.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Compliance wi
4、th a British Standard cannot confer immunityfrom legal obligations.0 SeptemberEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 3451-1August 2008ICS 83.080.01 Supersedes EN ISO 3451-1:1997 English VersionPlastics - Determination of ash - Part 1: General methods (ISO3451-1:2008)Plastiques - Dterm
5、ination du taux de cendres - Partie 1:Mthodes gnrales (ISO 3451-1:2008)Kunststoffe - Bestimmung der Asche - Teil 1: AllgemeineGrundlagen (ISO 3451-1:2008)This European Standard was approved by CEN on 26 July 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipula
6、te 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 may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exist
7、s 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 CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodie
8、s of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEA
9、N COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 3451-1:2008: EBS EN ISO 3451-1
10、:2008EN ISO 3451-1:2008 (E) 3 Foreword This document (EN ISO 3451-1:2008) has been prepared by Technical Committee ISO/TC 61 “Plastics“ in collaboration with Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. This European Standard shall be given the status of a natio
11、nal standard, either by publication of an identical text or by endorsement, at the latest by February 2009, and conflicting national standards shall be withdrawn at the latest by February 2009. Attention is drawn to the possibility that some of the elements of this document may be the subject of pat
12、ent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 3451-1:1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this Euro
13、pean Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United
14、 Kingdom. Endorsement notice The text of ISO 3451-1:2008 has been approved by CEN as a EN ISO 3451-1:2008 without any modification. BS EN ISO 3451-1:2008ISO 3451-1:2008(E) ISO 2008 All rights reserved iiiContents Page Foreword iv 1 Scope1 2 Normative references1 3 Terms and definitions .1 4 Principl
15、e .2 5 Reagents (for methods B and C only).2 6 Apparatus.2 7 Procedure.3 7.1 Test portion3 7.2 Test conditions3 7.3 Method A Direct calcination 4 7.4 Method B Calcination following sulfuric acid treatment after burning .4 7.5 Method C Calcination following sulfuric acid treatment before burning5 8 N
16、umber of tests .5 9 Expression of results5 10 Precision 5 11 Test report6 BS EN ISO 3451-1:2008ISO 3451-1:2008(E) iv ISO 2008 All rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of p
17、reparing International Standards 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,
18、in liaison with ISO, also take 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 ta
19、sk of technical committees is 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. Attenti
20、on is drawn to the possibility 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 3451-1 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical pro
21、perties. This fourth edition cancels and replaces the third edition (ISO 3451-1:1997), which has been technically revised, in particular with respect to the mass of the test portion used (see 7.1). ISO 3451 consists of the following parts, under the general title Plastics Determination of ash: Part
22、1: General methods Part 2: Poly(alkylene terephthalate) materials Part 3: Unplasticized cellulose acetate Part 4: Polyamides Part 5: Poly(vinyl chloride) BS EN ISO 3451-1:2008INTERNATIONAL STANDARD ISO 3451-1:2008(E) ISO 2008 All rights reserved 1Plastics Determination of ash Part 1: General methods
23、 SAFETY STATEMENT Persons using this document should be familiar with normal laboratory practice, if applicable. This document does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health prac
24、tices and to ensure compliance with any regulatory requirements. 1 Scope This part of ISO 3451 specifies general methods, with suitable test conditions, for the determination of the ash of a range of plastics (resins and compounds). The particular conditions chosen may be included in the specificati
25、ons for the plastic material in question. Particular conditions applicable to poly(alkylene terephthalate) materials, unplasticized cellulose acetate, polyamides and poly(vinyl chloride) plastics, including some specific filled, glass-fibre-reinforced and flame-retarded materials, are specified in I
26、SO 3451-2, ISO 3451-3, ISO 3451-4 and ISO 3451-5. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including a
27、ny amendments) applies. ISO 472, Plastics Vocabulary 3 Terms and definitions For the purposes of this document, the terms and definitions given in ISO 472 apply. BS EN ISO 3451-1:2008ISO 3451-1:2008(E) 2 ISO 2008 All rights reserved4 Principle It is possible to determine the ash of an organic materi
28、al by three main methods: a) Direct calcination, i.e. by burning the organic matter and heating the residue at high temperature until constant mass is reached (method A). b) Calcination after sulfation, which may be carried out by two different procedures: With sulfuric acid treatment after burning,
29、 i.e. by burning the organic matter, transforming the inorganic residue into sulfates with concentrated sulfuric acid and heating the residue at high temperature until constant mass is reached. This is the common method of obtaining “sulfated ash” (method B). With sulfuric acid treatment before burn
30、ing, i.e. by heating the organic matter together with concentrated sulfuric acid up to temperatures where fuming and subsequent burning of the organic matter occur, and finally heating the residue at high temperature until constant mass is reached (method C). This procedure may be used if volatile m
31、etal halides are liable to evaporate during burning of the organic matter. It is not applicable to silicones or fluorine-containing polymers. In each case, the final step of the procedure is calcination at 600 C, 750 C, 850 C or 950 C until constant mass is reached (see 7.2). NOTE The mass of the as
32、h may vary with the temperature of ignition. For example, higher temperatures such as 850 C will convert calcium carbonate and other carbonates to their oxides and thus give lower values for the ash. 5 Reagents (for methods B and C only) During the analysis, use only reagents of analytical grade and
33、 only distilled water or water of equivalent purity. 5.1 Ammonium carbonate, anhydrous. 5.2 Ammonium nitrate, approximately 10 % (by mass) solution. 5.3 Sulfuric acid, = 1,84 g/cm3. WARNING Highly corrosive. Handle with suitable skin and eye protection in a fume cupboard. Reacts exothermically with
34、water. 5.4 Sulfuric acid, 50 % (by volume) solution. WARNING Handle with care. Prepare by slowly adding the concentrated acid to water. 6 Apparatus 6.1 Crucible, made of silica, porcelain or platinum, inert to the material tested. The use of a crucible lid/watch-glass may be beneficial for samples p
35、roducing a fine particulate ash. 6.2 Gas burner, or other appropriate heat source. 6.3 Muffle furnace or microwave furnace, capable of being maintained at 600 C 25 C, 750 C 50 C, 850 C 50 C or 950 C 50 C, as appropriate. 6.4 Analytical balance, accurate to 0,1 mg. 6.5 Pipettes, of suitable capacity
36、(for methods B and C only). BS EN ISO 3451-1:2008ISO 3451-1:2008(E) ISO 2008 All rights reserved 36.6 Desiccator, containing an efficient desiccant which does not interact with the ash. NOTE In certain cases, the ash may have a greater affinity for water than some substances commonly used as desicca
37、nts. 6.7 Weighing bottle. 6.8 Fume cupboard. 7 Procedure 7.1 Test portion Take a quantity of the test sample sufficient to yield 5 mg to 500 mg of ash (see Table 1). In the case of reinforced materials, take a test portion of 2 g. If the likely quantity of ash is unknown, carry out a preliminary ash
38、 determination. Depending on the approximate ash content, choose the size of the test portion to be used from Table 1. Table 1 Mass of test portion Approximate ash % Test portion g Mass of ash obtained mg u 0,01 W 200 approximately 5 to 10 0,01 to 0,05 100 10 to 50 0,05 to 0,1 50 25 to 50 0,1 to 0,2
39、 25 25 to 50 0,2 to 1 10 20 to 100 1 to 10 5 50 to 500 10 2 200 For plastics yielding very low ash, it is necessary to use larger test portions. When it is impossible to burn the whole of the test portion at one time, weigh the required quantity in a suitable weighing bottle and introduce it into th
40、e crucible (6.1) in convenient amounts for a succession of burnings until the whole of the test portion has been burnt. 7.2 Test conditions Calcination shall be continued to constant mass as defined in 7.3.6, but the duration of the calcination in the muffle furnace (6.3) shall not exceed 3 h at the
41、 specified temperature. The choice of the calcination temperature and the use of the sulfation method depend on the nature of the plastic and any additives it may contain. If a choice exists between different satisfactory conditions, choose those that allow the attainment of constant mass in less th
42、an 3 h. A higher temperature or the use of sulfation generally shortens the duration of the calcination. Whichever method A, B or C is used, choose one of the following temperature ranges for the final (calcination) step, unless other temperatures are requested for special technical or commercial re
43、asons: 600 C 25 C, 750 C 50 C, 850 C 50 C, 950 C 50 C. Use a fume cupboard for the ashing procedure. BS EN ISO 3451-1:2008ISO 3451-1:2008(E) 4 ISO 2008 All rights reservedFor method A, if it can be conclusively demonstrated for a particular sample type that direct ashing in a muffle furnace without
44、preheating/igniting the sample over a Bunsen flame or equivalent gives the same result, then this version of method A (rapid ashing) is permitted. The use of this rapid ashing method shall be included in the test report. 7.3 Method A Direct calcination 7.3.1 Prepare the crucible (6.1) by heating it
45、in the muffle furnace (6.3) at the test temperature until constant mass is reached. Allow to cool in the desiccator (6.6) to room temperature for 1 h, or until room temperature is reached, and weigh on the analytical balance (6.4) to the nearest 0,1 mg. 7.3.2 Introduce into the tared weighing bottle
46、 (6.7) a test portion (pre-dried as described in the corresponding material specification) of mass in accordance with Table 1. Weigh again to the nearest 0,1 mg or to 0,1 % of the mass of the test portion. If the test portion corresponding to the amount of ash specified in Table 1 does not more than
47、 half fill the crucible, this quantity may be placed directly into the crucible and weighed in it. The procedure described below assumes that this will not be the case, however. High-bulk materials may be compressed into tablets, which may then be broken up into fragments of appropriate size. 7.3.3
48、Introduce into the crucible enough of the test portion to half fill the crucible. Heat the crucible directly on the burner or other suitable heating device (6.2) to burn slowly until volatile products have been driven off. Repeat the operation until the whole test portion is well charred. 7.3.4 Intr
49、oduce the crucible into the muffle furnace preheated to the prescribed temperature and calcine for 30 min. 7.3.5 Place the crucible in the desiccator, allow it to cool for 1 h, or until room temperature is reached, and weigh on the analytical balance to the nearest 0,1 mg. 7.3.6 Calcine again under the same conditions until constant mass is reached, i.e. until the results of two consecutive weighings do not differ from each other by more than 0,5 mg. 7.3.7 If a laboratory
