1、Adhesives English version of DIN EN 1246 Determination of ash and sulphated ash ICs 83.180 DIN EN 1246 - Descriptors: Adhesives, ash content, analysis. Klebstoffe - Bestimmung des Aschegehaltes und des Sulfat- Aschegehaltes European Standard EN 1246 : 1998 has the status of a DIN Standard. A comma i
2、s used as the decimal marker. National foreword This standard has been prepared by CEN/TC 193. The responsible German body involved in its preparation was the Normenausschu Kunststoffe (Plastics Standards Committee), Technical Committee Klebstoffe - Terminologie; physikalisch-chemische Prfungen. EN
3、comprises 6 pages. No pari of this standard may be reproduced without the prior permission of Ref. No. DIN EN 1246: 1998-0 V Deutsches Institut fr Nonung e. V., Berlin. Luth Verlag GmbH, D-10772 Berlin, has the exclusive right of sale for German Standards (DIN-Normen). English price group 06 . Sales
4、 No . . 1106 10.98 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1246 February 1998 ICs 83.180 Descriptors: Adhesives, ash content, analysis. English version Adhesives Determination of ash and sulphated ash Adhsifs - Dtermination du taux de cendres total et du taux de cendres sulfates Aschege
5、haltes Klebstoffe - Bestimmung des Aschegehaltes und des Sulfat- This European Standard was approved by CEN on 1998-01 -24. CEN members are bound to comply with the CENKENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard with
6、out any alteration. Up-to-date lists and bibliographical references concerning such national stand- ards may be obtained on application to the Central Secretariat or to any CEN member. The European Standards exist in three official versions (English, French, German). A version in any other language
7、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 members are the national standards bodies of Austria, Belgium, the Czech Republic, Denmark, Finland, France, Germany, Greece, I
8、celand, Ireland, Italy, Luxembourg, the Netherlands, Norway, Portugal, Spain, Sweden, Switzerland, and the United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, 8-1050 Brussels O 1998. CEN - A
9、ll rights of exploitation in any form and by any means reserved worldwide for CEN national members. Ref. No. EN 1246 : 1998 E Page 2 EN 1246: 1998 Foreword This European Standard has been prepared by Technical Committee CEN/TC 193 llAdhesivesll, the secretariat of which is held by AENOR . This Europ
10、ean 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 1998, and conflicting national standards shall be withdrawn at the latest by August 1998. According to the CEN/CENELEC Internal Regulations, the nation
11、al 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, Spain, Sweden, Switzerland and the United Kingdom. 1 S
12、cope This European Standard specifies two conventional methods for the determination of ash and sulphated ash content of a synthetic or natural adhesive. 2 Normative references This European Standard incorporates, by dated or undated reference, provisions from other publications. These nonnative ref
13、erences are cited at the appropriate places in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references th
14、e latest edition of the publication referred to applies. EN 827 Adhesives - Determination of conventional solids content and constant mass solids content. EN 923 Adhesives - Terms and definitions. EN 1066 Adhesive - Sampling. EN 1067 Adhesives - Examination and preparation of samples for testing. IS
15、0 5725-2 Accuracy (trueness and precision) of measurement methods and results - Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method Page 3 EN 1246 : 1998 3 Definitions For the purposes of this standard, the definitions given in EN 923 appl
16、y. 4 Principle 4.1 Method A: Determination of the percentage of ash Preliminary drying and combustion of the test sample and ashing in a muffle furnace at prefixed temperature to constant mass. 4.2 Method B: Determination of the percentage of ash as sulpha t es Preliminary combustion of the test sam
17、ple, treatment of the residue with sulphuric acid, heating, neutralization of excess acid by the addition of ammonium carbonate and heating. Then ashing in a muffle furnace at prefixed temperature to constant mass. 5 Safety Persons using this standard shall be familiar with normal laboratory practic
18、e. This standard does not purport to address all safety problems, 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 European and national regulatory conditions. 6 Reagents (used only for sulpha
19、ted ash) 6.1 Sulphuric acid, pure, p 1,84 g/ml; 6.2 grade, Ammonium carbonate , anhydrous , powdered, analytical reagent 7 Appara tu8 7.1 Crucibles, of silica, porcelain or platinum 45 mm to 75 mm diameter and a depth not less than the length of the diameter. Deep crucibles are particulary recommend
20、ed especially for the determination of sulphated ash. 7.2 Bunsen burner or equivalent apparatus; 7.3 Muffle furnace gas or electric, controlled at (850 f 20) “C; Page 4 EN 1246 : 1998 7.4 Oven, adjustable between 80 OC and 135 OC; 7.5 Analytical balance accurate to 0,0001 g; 7.6 Desiccator containin
21、g conventional desiccant; 7.7 Pipette. 8 Sampling A significant sample of the adhesive shall be taken in accordance with EN 1066 and prepared for testing in accordance with EN 1067. 9 Procedure Carry out the following procedure in duplicate: Calculate the mass m, in grams of ash from the difference
22、in the weighings. Calculate the mass %, in grams of sulphated ash from the difference in the weighings. 9.1 Method A: Determination of the percentage of ash 9.1.1 Heat the crucible (see 7.l)at (850 f 20) “C to constant mass and cool in the desiccator (see 7.6). Weigh the crucible to the nearest O, 0
23、005 g and add 2 g to 3 g of adhesive. Reweigh the crucible and its content to the nearest O, 0005 g and calculate the mass mo of the adhesive used. 9.1.2 Dry in the oven (see 7.4) under the same conditions as those used to measure the conventional solids content in accordance with EN 827 for the adh
24、esive involved. Solid adhesives do not require this operation. 9.1.3 Gently heat the crucible with the Bunsen burner (see 7.2), or equivalent apparatus, until all volatile matter and any other products of combustion are completely volatized. This is indicated by the disappearance of the black colour
25、 from the inside walls of the crucible. The ashing shall be carried out slowly so that the volatiles do not carry off particles of ash. 9.1.4 Place the crucible in the muffle furnace (see 7.3) controlled at (850 f 20) “C and heat for 10 min. Page 5 EN 1246 : 1998 After cooling in the desiccator, wei
26、gh the crucible to the nearest 0,0005 g. Heat again for 10 min, recool in the desiccator and reweigh. Repeat these operations until constant mass is obtained i.e. until two successive weighings do not differ by more than 0,0005 g. 9.2 Method B: Determination of the percentage of sulphated ash 9.2.1
27、Heat the crucible (see 7.1) at (850 f 20) “C to constant mass and cool in the desiccator (see 7.6). Weigh the crucible to the nearest 0,0005 g and add 2 g to 3 g of adhesive. Reweigh the crucible and its contents to the nearest 0,0005 g and calculate the mass m, of the adhesive used. 9.2.2 Dry in th
28、e oven (see 7.4) under the same conditions as those used to measure the conventional solids content in accordance with EN 827 for the adhesive involved. Solid adhesives do not require this operation. 9.2.3 Gently heat the crucible with the Bunsen burner (see 7.2) or equivalent apparatus until all vo
29、latile matter and any other products of combustion are completely volatized. This stage is indicated by the disappearance of the black colour from the inside walls of the crucible. The ashing shall be carried out slowly so that the volatiles do not carry off particles of ash. 9.2.4 Allow the crucibl
30、e and contents to cool. By means of the pipette (see 7.7) add to the crucible successive small quantities of sulphuric acid (see 6.1) warming carefully with the bunsen burner (see 7.2) until the reaction is completed. Then, add ammonium carbonate (see 6.2) to neutralize excess acid, warming until th
31、e emission of white fumes ceases. 9.2.5 Place the crucible in the muffle furnace (see 7.3) controlled at (850 f 20) OC and heat for 10 min. After cooling in the desiccator, weigh the crucible to the nearest 0,0005 g. Heat again for 10 min, recool in the desiccator and reweigh. Repeat these operation
32、s until constant mass is obtained i.e. until two successive weighings do not differ by more than 0,0005 g. Page 6 EN 1246: 1998 10 Expression of results For each determination calculate the percentage of ash or sulphated ash to two decimal places by means of the formulae: sulphated ash % = msl - 100
33、 m0 where : m, is the mass, in grams, of adhesive used; m, is the mass, in grams, of ash; Q, is the mass, in grams, of sulphated ash. Calculate the mean to the nearest 0,0005 grams of the two values finally obtained. In the test report include the mean as the value of the percentage of ash or sulpha
34、ted ash. 11 Precision a) Repeatability (in accordance with IS0 5725-2): 0,10% b) Reproducibility (in accordance with IS0 5725-2): 0,20% 12 Test report The test report shall include: a) a reference to this draft European Standard; b) the type and designation of the adhesive tested; c) the result of the test expressed in accordance with clause 10; d) any circumstances which may have affected the result; e) date of test.
