1、November 2008DEUTSCHE NORM English price group 8No part of this standard may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 83.080.01!$Rdq“1476578
2、www.din.deDDIN EN ISO 3451-1Plastics Determination of ash Part 1: General methods (ISO 3451-1:2008)English version of DIN EN ISO 3451-1:2008-11Kunststoffe Bestimmung der Asche Teil 1: Allgemeine Grundlagen (ISO 3451-1:2008)Englische Fassung DIN EN ISO 3451-1:2008-11SupersedesDIN EN ISO 3451-1:1997-1
3、0www.beuth.deDocument comprises 11 pagesDIN EN ISO 3451-1:2008-11 2 National foreword This standard has been prepared by Technical Committee ISO/TC 61 “Plastics” in collaboration with Technical Committee CEN/TC 249 “Plastics”, (Secretariat: NBN, Belgium). The responsible German body involved in its
4、preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Technical Committee NA 054-01-03 AA Physikalische, rheologische und analytische Prfungen. The DIN Standard corresponding to the International Standard referred to in this document is as follows: ISO 472 DIN EN ISO 472 Am
5、endments This standard differs from DIN EN ISO 3451-1:1997-10 as follows: a) The standard has been editorially revised. b) Clause 2 “Normative references” has been updated, clause 3 “Terms and definitions” has been added and subsequent clauses have been renumbered. c) Tables 1 and 2 have been extend
6、ed. Previous editions DIN ISO 3451-1: 1991-04 DIN EN ISO 3451-1: 1997-10 National Annex NA (informative) Bibliography DIN EN ISO 472, Plastics Vocabulary EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN ISO 3451-1August 2008ICS 83.080.01 Supersedes EN ISO 3451-1:1997 English VersionPlastiques - Dte
7、rmination 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 stipu
8、late 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 exi
9、sts 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 bod
10、ies 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.EUROP
11、EAN 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: EPlastics - Det
12、ermination of ash - Part 1: General methods(ISO 3451-1:2008)Contents Page 1 2 3 4 5 6 7 7.1 7.2 7.3 7.4 7.5 8 9 10 11 2 DIN EN ISO 3451-1:2008-11 EN ISO 3451-1:2008 (E)Foreword .3 Scope4 Normative references4 Terms and definitions .4 Principle .5 Reagents (for methods B and C only).5 Apparatus.5 Pro
13、cedure.6 Test conditions6 Test portion6 Method A Direct calcination 7 Method C Calcination following sulfuric acid treatment before burning8 Method B Calcination following sulfuric acid treatment after burning .7 Number of tests .8 Expression of results8 Precision 8 Test report9 Foreword This docume
14、nt (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 national standard, either by publication of an identica
15、l 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 patent rights. CEN and/or CENELEC shall not be held r
16、esponsible 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 European Standard: Austria, Belgium, Bulgaria, Cyprus,
17、 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 Kingdom. Endorsement notice The text of ISO 3451-
18、1:2008 has been approved by CEN as a EN ISO 3451-1:2008 without any modification. 3 DIN EN ISO 3451-1:2008-11 EN ISO 3451-1:2008 (E)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 saf
19、ety concerns, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any regulatory requirements. 1 Scope This part of ISO 3451 specifies general methods, with suitable test conditions, for the determin
20、ation of the ash of a range of plastics (resins and compounds). The particular conditions chosen may be included in the specifications for the plastic material in question. Particular conditions applicable to poly(alkylene terephthalate) materials, unplasticized cellulose acetate, polyamides and pol
21、y(vinyl chloride) plastics, including some specific filled, glass-fibre-reinforced and flame-retarded materials, are specified in ISO 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 d
22、ated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any 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. 4 DIN E
23、N ISO 3451-1:2008-11 EN ISO 3451-1:2008 (E)4 Principle It is possible to determine the ash of an organic material 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 aft
24、er sulfation, which may be carried out by two different procedures: With sulfuric acid treatment after burning, 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 reac
25、hed. This is the common method of obtaining “sulfated ash” (method B). With sulfuric acid treatment before burning, 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
26、residue at high temperature until constant mass is reached (method C). This procedure may be used if volatile metal 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 i
27、s calcination at 600 C, 750 C, 850 C or 950 C until constant mass is reached (see 7.2). NOTE The mass of the ash 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 fo
28、r the ash. 5 Reagents (for methods B and C only) During the analysis, use only reagents of analytical grade and 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
29、 Highly corrosive. Handle with suitable skin and eye protection in a fume cupboard. Reacts exothermically with 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 o
30、r platinum, inert to the material tested. The use of a crucible lid/watch-glass may be beneficial for samples producing 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
31、 or 950 C 50 C, as appropriate. 6.4 Analytical balance, accurate to 0,1 mg. 6.5 Pipettes, of suitable capacity (for methods B and C only). 5 DIN EN ISO 3451-1:2008-11 EN ISO 3451-1:2008 (E)6.6 Desiccator, containing an efficient desiccant which does not interact with the ash. NOTE In certain cases,
32、the ash may have a greater affinity for water than some substances commonly used as desiccants. 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
33、 test portion of 2 g. If the likely quantity of ash is unknown, carry out a preliminary ash 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,
34、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 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 o
35、ne time, weigh the required quantity in a suitable weighing bottle and introduce it into the 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,
36、but the duration of the calcination in the muffle furnace (6.3) shall not exceed 3 h at the 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
37、satisfactory conditions, choose those that allow the attainment of constant mass in less than 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 (calcin
38、ation) step, unless other temperatures are requested for special technical or commercial reasons: 600 C 25 C, 750 C 50 C, 850 C 50 C, 950 C 50 C. Use a fume cupboard for the ashing procedure. 6 DIN EN ISO 3451-1:2008-11 EN ISO 3451-1:2008 (E)For method A, if it can be conclusively demonstrated for a
39、 particular sample type that direct ashing in a muffle furnace without 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 Meth
40、od A Direct calcination 7.3.1 Prepare the crucible (6.1) by heating it 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
41、) to the nearest 0,1 mg. 7.3.2 Introduce into the tared weighing bottle (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 cor
42、responding to the amount of ash specified in Table 1 does not more than 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,
43、 which may then be broken up into fragments of appropriate size. 7.3.3 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
44、 the operation until the whole test portion is well charred. 7.3.4 Introduce 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 t
45、he 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 can document that their procedure for time and tempe
46、rature of a single calcination on a given material results in constant mass, then this so-called “rapid method” shall be permitted and the test report shall note a single calcination. In the event of a dispute, the referee method shall be calcination to constant mass. 7.4 Method B Calcination follow
47、ing sulfuric acid treatment after burning 7.4.1 Proceed as specified in 7.3.1, 7.3.2 and 7.3.3. 7.4.2 After cooling, add sulfuric acid solution (5.4) drop by drop with a pipette of suitable capacity (6.5) to moisten the residue completely and heat until fuming ceases, avoiding too vigorous boiling.
48、7.4.3 If traces of carbonaceous materials remain after cooling, add 1 to 5 drops of ammonium nitrate solution (5.2) and heat until the evolution of white fumes ceases completely. 7.4.4 In order to reconvert metal oxides formed during the preceding steps into sulfates, add, after cooling, about 5 dro
49、ps of concentrated sulfuric acid (5.3) and heat until there is no further evolution of white fumes, avoiding vigorous boiling or the loss of ash by excessive fuming. 7.4.5 After cooling, add 1 g to 2 g of solid ammonium carbonate (5.1) and heat, avoiding loss of ash, until the fuming has ceased. Then place the crucible in the muffle furnace preheated to the indicated temperature and proceed as specified in 7.3.4, 7.3.5 and 7.3.6. 7 DIN EN ISO 3451-1:2008-11 EN ISO 3451-1:2008 (E)7.5 Method C Calcina
