DIN EN 1428-2012 Bitumen and bituminous binders - Determination of water content in bituminous emulsions - Azeotropic distillation method German version EN 1428 2012《沥青和沥青粘合剂 沥青乳剂中.pdf

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1、March 2012Translation by DIN-Sprachendienst.English price group 8No part of this translation 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 75

2、.140; 91.100.50!$za“1876296www.din.deDDIN EN 1428Bitumen and bituminous binders Determination of water content in bituminous emulsions Azeotropic distillation methodEnglish translation of DIN EN 1428:2012-03Bitumen und bitumenhaltige Bindemittel Bestimmung des Wassergehaltes von Bitumenemulsionen Az

3、eotropisches DestillationsverfahrenEnglische bersetzung von DIN EN 1428:2012-03Bitumes et liants bitumineux Dtermination de la teneur en eau dans les mulsions de bitume Mthode de distillation azotropiqueTraduction anglaise de DIN EN 1428:2012-03SupersedesDIN EN 1428:1999-12www.beuth.deIn case of dou

4、bt, the German-language original shall be considered authoritative.Document comprises 11 pages02.12 DIN EN 1428:2012-03 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 336 “Bituminous binders” (Secretariat: AFNOR, France). The

5、responsible German bodies involved in its preparation were the Normenausschuss Materialprfung (Materials Testing Standards Committee) and the Normenausschuss Bauwesen (Building and Civil Engineer-ing Standards Committee), Joint Committee NA 062-03-32 GA Bitumen; Prfverfahren und Anforderungen fr die

6、 Bindemittel. The DIN Standard corresponding to the European Standard referred to in this document is as follows: EN ISO 3696 DIN ISO 3696 Amendments This standard differs from DIN EN 1428:1999-12 as follows: a) The standard has been editorially revised. Previous editions DIN 1995: 1929, 1934, 1941-

7、11, 1960x-02, 1980-12 DIN 52048: 1980-12 DIN EN 1428: 1999-12 National Annex NA (informative) Bibliography DIN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 1428 January 2012 ICS 75.140; 91.100.50 Supersed

8、es EN 1428:1999English Version Bitumen and bituminous binders - Determination of water content in bituminous emulsions - Azeotropic distillation methodBitumes et liants bitumineux - Dtermination de la teneur en eau dans les mulsions de bitume - Mthode de distillation azotropique Bitumen und bitumenh

9、altige Bindemittel - Bestimmung des Wassergehaltes von Bitumenemulsionen - Azeotropisches Destillationsverfahren This European Standard was approved by CEN on 20 November 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this Eu

10、ropean 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 CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versi

11、ons (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 CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria,

12、Belgium, Bulgaria, Croatia, 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, Turkey and United Kingdom. M

13、anagement Centre: Avenue Marnix 17, B-1000 Brussels 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 1428:2012: EEUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGEN 1428:2012 (E)

14、 2 Contents Page Foreword 31 Scope 42 Normative references 43 Terms and definitions .44 Principle 45 Reagents and materials 46 Apparatus .57 Sampling .78 Procedure .79 Calculation 710 Expression of results 811 Precision .812 Test report 8Annex A (normative) Verification of apparatus 9DIN EN 1428:201

15、2-03 EN 1428:2012 (E) 3 Foreword This document (EN 1428:2012) has been prepared by Technical Committee CEN/TC 336 “Bituminous binders”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by

16、 endorsement, at the latest by July 2012, and conflicting national standards shall be withdrawn at the latest by July 2012. 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 responsible for ident

17、ifying any or all such patent rights. This document supersedes EN 1428:1999. 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, Croatia, Cyprus, Czech Republic,

18、Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 1428:2012-03 EN 1428:2012 (E) 4 1 Scope Th

19、is European Standard specifies a method for the determination of the water content in bituminous emulsions by means of distillation. WARNING The use of this standard may involve hazardous materials, operations and equipment. This standard does not purport to address all of the safety problems associ

20、ated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2 Normative references The following referenced documents are indispensable for the application of thi

21、s document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 58, Bitumen and bituminous binders Sampling bituminous binders EN 12594, Bitumen and bituminous binders Preparation of test s

22、amples EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696) ISO 5272, Toluene for industrial use Specifications ISO 5280, Xylene for industrial use Specification 3 Terms and definitions For the purposes of this document, the following terms and definitions apply

23、. 3.1 water content mass percentage of water determined in accordance with the method specified in this standard 4 Principle The water contained in a bituminous emulsion is distilled over by means of a carrier vapour from a water immiscible solvent-carrier liquid. Condensed solvent-carrier liquid an

24、d water are separated continuously in a graduated receiver; the water settles in the graduated section of the receiver and the condensed solvent-carrier liquid returns to the flask. 5 Reagents and materials Use only reagents of recognized analytical grade and water conforming to grade 3 of EN ISO 36

25、96. 5.1 Distillation regulators, with a higher density than the liquid under test such as, for instance, anhydrous anti-bumping granules (e.g. boiling sand), glass beads. 5.2 Suitable solvent-carrier liquid. DIN EN 1428:2012-03 EN 1428:2012 (E) 5 Xylene conforming to ISO 5280 is recommended for rout

26、ine tests. Other petroleum distillates, conforming to the following distillation requirements: 98% distils between 120C and 250C, are suitable. In the event of dispute, toluene conforming to ISO 5272 shall be used. NOTE In selecting a solvent-carrier liquid, attention is drawn to any relevant safety

27、 regulations. 6 Apparatus Usual laboratory apparatus and glassware, together with the following: 6.1 Distillation apparatus (see Figure 1) consisting of the following: flask, receiver and condenser being connected with suitable ground glass joints. 6.1.1 Flask, 500 ml round bottomed with a short nec

28、k capable of supporting the reflux tube on the receiver. 6.1.2 Receiver, with a 25 ml nominal capacity graduated to 0,1 ml. 6.1.3 Vertical condenser, water-cooled with a minimum length of jacket of 300 mm. 6.1.4 Heater. NOTE An electric flask heater with electronic power regulation is recommended in

29、 order to obtain controlled distillation. DIN EN 1428:2012-03 EN 1428:2012 (E) 6 Dimension in millimetres 1. Reflux condenser 2. Receiver a With or without this tube b Capacity: 25 ml 3. Round bottomed flask Figure 1 Typical assembly 6.2 Stainless steel wire, with looped-end or fitted with a rubber

30、stopper. NOTE Other materials or devices are acceptable provided they allow dislodging the water (8.2.7) without interfering with the measurement. DIN EN 1428:2012-03 EN 1428:2012 (E) 7 6.3 Balance, of sufficient capacity, accurate to 0,01 g. 7 Sampling The test material shall be sampled in accordan

31、ce with EN 58. Preparation of test samples shall be made in accordance with EN 12594. The prepared sample shall be divided into two test portions. For referee purposes, both portions shall be tested (see Clause 10, 2ndparagraph). 8 Procedure 8.1 Verification of apparatus When necessary the apparatus

32、 shall be verified in accordance with the procedure given in Annex A. The verification procedure shall be carried out on new apparatus before using it for the first time and existing apparatus shall be checked annually. 8.2 Test 8.2.1 Carry out the procedure under normal laboratory conditions, at a

33、temperature of (23 5) C. 8.2.2 Before commencing a test, ensure that the distillation apparatus is clean and dry. 8.2.3 Pour 100 ml to 200 ml of solvent-carrier liquid (5.2) added with distillation regulator (5.1) into the round bottomed flask (6.1.1). 8.2.4 Weigh a sample of the emulsion under test

34、, of such a size that the distillation of 15 ml to 25 ml of water can be expected, into the round bottomed flask (6.1.1). NOTE Adequate measures should be taken so as to prevent splashes of emulsion onto the neck of the flask, (e.g. rod, funnel, .). 8.2.5 Assemble the apparatus and insert a loose pl

35、ug of cotton wool in the top of the condenser tube (6.1.3) to prevent the condensation of atmospheric moisture in the condenser tube. 8.2.6 Heat the flask to boiling point, adjusting the rate of boiling so that condensate falls from the end of the condenser at a rate of two to five drops per second.

36、 8.2.7 If there is water in the condenser tube or adhering to the sides of the receiver, dislodge it with the stainless steel wire (6.2). Continue distillation until the volume of water in the receiver is constant and no water is visible other than in the receiver. 8.2.8 Rinse the condenser with sol

37、vent-carrier liquid (5.2) from a wash bottle. 8.2.9 Allow a clear interface to develop between the water and solvent layers in the receiver then read off the volume of water to the nearest 0,1 ml. 9 Calculation Calculate the water content of the material under test (w), as a mass percentage, using t

38、he following equation: DIN EN 1428:2012-03 EN 1428:2012 (E) 8 100 x EmWmw = where Wm is the mass of the water distilled from the test material, in grams, and is equal to the volume of water, in millilitres collected in the graduated receiver; Em is the mass of emulsion used for the test, in grams. 1

39、0 Expression of results Express the water content as a mass percentage to the nearest 0,1 % or, for referee purposes, as the arithmetic mean of two tests. Duplicate tests are required for referee purposes only. In the case of routine internal production control, it is permitted to perform a single t

40、est. 11 Precision 11.1 Repeatability The difference between two test results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material would, in the long term, in the normal and correct operation of the test method, exceed 1 % mass fraction

41、 in absolute value, in only one case in twenty. 11.2 Reproducibility The difference between two single and independent results obtained by different operators working in different laboratories on identical test material would, in the long run, in the normal and correct operation of the test method,

42、exceed 2 % mass fraction in absolute value, in only one case in twenty. In the case of an emulsion containing a flux, the reproducibility is 3 % mass fraction in absolute value. 12 Test report The test report shall contain at least the following information: a) type and complete identification of th

43、e sample under test; b) reference to this European Standard; c) type of solvent used; d) result of the test (see Clause 10); e) number of tests performed; f) any deviation, by agreement or otherwise, from the procedure specified; g) date of the test. DIN EN 1428:2012-03 EN 1428:2012 (E) 9 Annex A (n

44、ormative) Verification of apparatus A.1 A given apparatus assembly shall be considered satisfactory if a result within permissible limits is obtained after a known quantity of water (5) is added to the solvent-carrier liquid (5.2) and the mixture is tested in accordance with 8.2. A.2 The results sha

45、ll be judged acceptable if the permissible limits given in Clause A.3 for the 25 ml graduated receiver are not exceeded. Results outside the permissible limits shall be investigated and the causes eliminated before proceeding. Repeat the verification until a result within the permissible limits is o

46、btained. A.3 The quantity (qw) of water added to the flask at ambient temperature shall be (15,00 0,02) g to (25,00 0,02) g. The permissible limits of water recovered at ambient temperature are qw 1,66 %. NOTE For this procedure, 1 ml of water may be taken as having a mass of 1 g. DIN EN 1428:2012-03