BS EN 1246-1998 Adhesives - Determination of ash and sulfated ash《胶粘剂 灰分和硫酸盐灰分的测定》.pdf

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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 1246:1998 The Europ

2、ean Standard EN 1246:1998 has the status of a British Standard ICS 83.180 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Adhesives Determination of ash and sulfated ashThis British Standard, having been prepared under the direction of the Sector Board for Materials and Chemic

3、als, was published under the authority of the Standards Board and comes into effect on 15 July 1998 BSI 1998 ISBN 0 580 29636 9 BS EN 1246:1998 Amendments issued since publication Amd. No. Date Text affected National foreword This British Standard is the English language version of EN 1246:1998. The

4、 UK participation in its preparation was entrusted to Technical Committee STI/52, Adhesives, which has the responsibility to: aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests in

5、formed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to

6、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 Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract

7、. 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 pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 4, an inside back cov

8、er and a back cover.CEN European Committee for Standardization Comite Europe en de Normalisation Europa isches Komitee fu r Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. R

9、ef. No. EN 1246:1998 E EUROPEAN STANDARD EN 1246 NORME EUROPE ENNE EUROPA ISCHE NORM February 1998 ICS 83.180 Descriptors: Adhesives, chemical analysis, ash determination, analysis methods English version Adhesives Determination of ash and sulfated ash Adhe sifs De termination du taux de cendres tot

10、al et du taux de cendres sulfate es Klebstoffe Bestimmung der Aschegehaltes und des Sulfat-Aschegehaltes This European Standard was approved by CEN on 24 January 1998. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European St

11、andard 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 member. This European Standard exists in three official versions (English, Frenc

12、h, 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 members are the national standards bodies of Austria, Belgium, Czech Republic, Denm

13、ark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.Page 2 EN 1246:1998 BSI 1998 Foreword This European Standard has been prepared by Technical Committee CEN/TC 193, Adhesives, the secretariat of whi

14、ch is held by AENOR. This 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 1998, and conflicting national standards shall be withdrawn at the latest by August 1998. According to the CEN/CENELEC I

15、nternal 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, Spain, Sweden, Switzerl

16、and and the United Kingdom.Page 3 EN 1246:1998 BSI 1998 1 Scope This European Standard specifies two conventional methods for the determination of ash and sulfated ash content of a synthetic or natural adhesive. 2 Normative references This European Standard incorporates, by dated or undated referenc

17、e, provisions from other publications. These normative references 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

18、 in it by amendment or revision. For undated references the 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

19、Examination and preparation of samples for testing. ISO 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. 3 Definitions For the purposes of this standard, the

20、definitions given in EN 923 apply. 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 a predetermined temperature to constant mass. 4.2 Method B: determination of the percentage of ash as sulfates Pr

21、eliminary combustion of the test sample, treatment of the residue with sulfuric acid, heating, neutralization of excess acid by the addition of ammonium carbonate and heating. Then ashing in a muffle furnace at a predetermined temperature to constant mass. 5 Safety Persons using this standard shall

22、be familiar with normal laboratory practice. 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 co

23、nditions. 6 Reagents (used only for sulfated ash) 6.1 Sulfuric acid, pure, r 1,84 g/ml. 6.2 Ammonium carbonate, anhydrous, powdered, analytical reagent grade. 7 Apparatus 7.1 Crucibles, of silica, porcelain or platinum,4 5m m to 75 mm diameter and a depth not less than the length of the diameter. De

24、ep crucibles are particulary recommended, especially for the determination of sulfated ash. 7.2 Bunsen burner or equivalent apparatus. 7.3 Muffle furnace, gas or electric, controlled at (850 20)8C. 7.4 Oven, adjustable between 808C and 1358C. 7.5 Analytical balance, accurate to 0,0001 g. 7.6 Desicca

25、tor, containing 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 1 in grams of ash from

26、the difference in the weighings. Calculate the mass m s1 in grams of sulfated ash from the difference in the weighings. 9.1 Method A: determination of the percentage of ash 9.1.1 Heat the crucible (see 7.1) at (850 20)8Ct o constant mass and cool in the desiccator (see 7.6). Weigh the crucible to th

27、e 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 0 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 8

28、27 for the adhesive 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 th

29、e 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.Page 4 EN 1246:1998 BSI 1998 9.1.4 Place the crucible in the muffle furnace (see 7.3) controlled at (850 20)8C and heat for 10 min. After cooling in th

30、e desiccator, weigh the crucible to the nearest 0,0005 g. Heat again for 10 min, re-cool 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 s

31、ulfated ash 9.2.1 Heat the crucible (see 7.1) at (850 20)8Ct o 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 0 of the adhesive used.

32、 9.2.2 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 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 appara

33、tus until all volatile 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 A

34、llow the crucible and contents to cool. By means of the pipette (see 7.7) add to the crucible successive small quantities of sulfuric 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,

35、warming until the emission of white fumes ceases. 9.2.5 Place the crucible in the muffle furnace (see 7.3) controlled at (850 20)8C and heat for 10 min. After cooling in the desiccator, weigh the crucible to the nearest 0,0005 g. Heat again for 10 min, re-cool in the desiccator and reweigh. Repeat t

36、hese operations until constant mass is obtained, i.e. until two successive weighings do not differ by more than 0,0005 g. 10 Expression of results For each determination calculate the percentage of ash or sulfated ash to two decimal places by means of the formulae: ash % = 3 100 m 1 m 0 sulfated ash

37、 % = 3 100 m s1 m 0 where: m 0 is the mass, in grams, of adhesive used; m 1 is the mass, in grams, of ash; m s1 is the mass, in grams, of sulfated 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 percentag

38、e of ash or sulfated ash. 11 Precision a) Repeatability (in accordance with ISO 5725-2): 0,10 % b) Reproducibility (in accordance with ISO 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;

39、 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.blankBSI 389 Chiswick High Road London W4 4AL | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | |

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