1、November 2015 English price group 9No 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 75.140; 91.100.50!%G(H“2360537ww
2、w.din.deDIN EN 12606-1Bitumen and bituminous binders Determination of the paraffin wax content Part 1: Method by distillation;English version EN 12606-1:2015,English translation of DIN EN 12606-1:2015-11Bitumen und bitumenhaltige Bindemittel Bestimmung des Paraffingehaltes Teil 1: Destillationsverfa
3、hren;Englische Fassung EN 12606-1:2015,Englische bersetzung von DIN EN 12606-1:2015-11Bitumes et liants bitumineux Dtermination de la teneur en paraffines Partie 1: Mthode par distillation;Version anglaise EN 12606-1:2015,Traduction anglaise de DIN EN 12606-1:2015-11SupersedesDIN EN 12606-1:2007-06w
4、ww.beuth.deDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.Document comprises 15 pages 09.15 DIN EN 12606-1:2015-11 2 A comma is used as the decimal marker. National foreword This document (EN 12606-1:2015) has been prepared by Tech
5、nical Committee CEN/TC 336 “Bituminous binders” (Secretariat: AFNOR, France). The responsible German bodies involved in its preparation were the DIN-Normenausschuss Materialprfung (DIN Standards Committee Materials Testing) and the DIN-Normenausschuss Bauwesen (DIN Standards Committee Building and C
6、ivil Engineering), Joint Committee NA 062-03-32 GA Bitumen; Prfverfahren und Anforderungen fr die Bindemittel. Amendments This standard differs from DIN EN 12606-1:2007-06 as follows: a) mercury thermometers are no longer given as the reference thermometer. The changes involve mainly the text in 6.2
7、; b) the standard has been editorially revised. Previous editions DIN 1995: 1929-01, 1934-01, 1941-11, 1960x-02 DIN 52015: 1980-12 DIN EN 12606-1: 2000-04, 2007-06 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 12606-1 July 2015 ICS 75.140; 91.100.50 Supersedes EN 12606-1:2007English Version B
8、itumen and bituminous binders - Determination of the paraffin wax content - Part 1: Method by distillation Bitumes et liants bitumineux - Dtermination de la teneur en paraffines - Partie 1 : Mthode par distillation Bitumen und bitumenhaltige Bindemittel - Bestimmung des Paraffingehaltes - Teil 1: De
9、stillationsverfahren This European Standard was approved by CEN on 27 May 2015. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bi
10、bliographical 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 versions (English, French, German). A version in any other language made by translation under the resp
11、onsibility 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, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Re
12、public of Macedonia, 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. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NOR
13、MALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 12606-1:2015 EEN 12606-1:2015 (E) 2 Contents Page Foreword 3 1 Scope 4
14、2 Normative references 4 3 Terms and definitions .4 4 Principle 4 5 Reagents and materials 5 6 Apparatus .5 7 Sampling .6 8 Procedure .6 9 Calculation 8 10 Expression of results 8 11 Precision .9 11.1 Repeatability .9 11.2 Reproducibility .9 12 Test report 9 13 Figures . 10 DIN EN 12606-1:2015-11 EN
15、 12606-1:2015 (E) 3 Foreword This document (EN 12606-1:2015) has been prepared by Technical Committee CEN/TC 336 “Bituminous binders”, the secretariat of which is held by AFNOR. This document supersedes EN 12606-1:2007. This European Standard shall be given the status of a national standard, either
16、by publication of an identical text or by endorsement, at the latest by January 2016, and conflicting national standards shall be withdrawn at the latest by January 2016. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or
17、CENELEC shall not be held responsible for identifying any or all such patent rights. The standard has been revised due to a normative reference to mercury thermometers. The changes involve mainly the text in 6.2. The terms “sample thermometer” and “bath thermometer” have been changed, as a consequen
18、ce, to “sample temperature transducer” and “bath temperature transducer” respectively in some subparagraphs of Clause 8. This draft European standard EN 12606 consists of the following parts under the general title Bitumen and bituminous binders Determination of the paraffin wax content Part 1: Meth
19、od by distillation; Part 2: Method by extraction. The changes introduced mainly involve the revision of the text in 6.2 relating to the mentioning of mercury thermometers as reference thermometers. According to the CEN/CENELEC Internal Regulations, the national standards organisations of the followi
20、ng countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Nor
21、way, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 12606-1:2015-11 EN 12606-1:2015 (E) 4 1 Scope This European Standard specifies a procedure for determining the paraffin wax content of bitumen and bituminous binder by the DIN method
22、. Aqueous bituminous binders, fluxed or cut-back anhydrous binders, and modified binders, whatever their consistency, are not within the scope of the present test method. WARNING Use of this European standard can involve hazardous materials, operations and equipment. This European standard does not
23、purport to address all of the safety problems associated with its use. It is the responsibility of the user of this European standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. 2 Normative references The following docu
24、ments, in whole or in part, are normatively referenced in this document and are indispensable for its application. 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 bitumi
25、nous binders - Sampling bituminous binders EN 1425, Bitumen and bituminous binders - Characterization of perceptible properties EN 12594, Bitumen and bituminous binders - Preparation of test samples EN ISO 3696:1995, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987
26、) ISO 383, Laboratory glassware Interchangeable conical ground joints 3 Terms and definitions For the purposes of this document, the following term and definition applies. 3.1 paraffin wax mixture of hydrocarbons crystallising in a 50 % volume fraction mixture of ether/ethanol at temperatures down t
27、o - 20 C, obtained by a specified process and having a melting range of above 25 C 4 Principle Paraffin wax present in bitumen is determined in the distillate obtained from a specified distillation process. DINEN 12606-1:2015-11EN 12606-1:2015 (E) 5 5 Reagents and materials 5.1 General Use only reag
28、ents of recognized analytical grade and water conforming to grade 3 of EN ISO 3696:1995 unless otherwise specified. 5.2 Ethoxyethane (Diethylether), anhydrous, referred to in this standard as ether. 5.3 Ethanol, absolute. 5.4 Ethanol, technical grade. 5.5 Petroleum spirit, with density of approximat
29、ely 645 kg/m at 15 C, and a distillation range of approximately 30 C to 75 C. 5.6 Acetone, reagent grade. 5.7 Carbon dioxide, solid, finely ground. NOTE A cryostat with a cooling effect equivalent to that of solid carbon dioxide can be used. 5.8 Ice, finely ground. 5.9 Washing liquid, a 50 % volume
30、fraction mixture of ether/ethanol. 6 Apparatus Usual laboratory apparatus and glassware, together with the following: (Dimensions in this clause are approximate unless tolerances are stated). 6.1 Oven, capable of maintaining (125 5) C. 6.2 Temperature measuring devices, (combining reading device and
31、 transducers) referred to in this standard as: 6.2.1 Sample temperature transducer: a sensor which together with a reading device shall have a measuring range of 38 C to 50 C, be readable to the nearest 1,0 C with an accuracy of 0,5 C. The sensor shall be embedded in a glass rod with total length (3
32、60 5) mm and outside diameter (10,0 0,5) mm. 6.2.2 Bath temperature transducer: a sensor which together with a reading device shall have a measuring range of 30 C to 50 C, be readable to the nearest 0,5 C with an accuracy of 0,5 C. The sensor shall be embedded in a glass rod with total length (220 5
33、) mm and outside diameter (8,0 0,5) mm. The temperature measuring devices employed shall be calibrated regularly. 6.3 Distillation flask as shown in Figure 1, fitted with cork stopper. 6.4 Sheet metal guard ring with an approximate 18 mm inside diameter and a 65 mm outside diameter. 6.5 Test tubes,
34、fitted with a spout and bored cork stopper; dimensions are given in Figure 2. 6.6 Test tubes, fitted with a 29/32 ground socket and a wash bottle fitted with a 29/32 ground cone according to ISO 383; dimensions are given in Figure 2. DIN EN 12606-1:2015-11 EN 12606-1:2015 (E) 6 6.7 Erlenmeyer flask,
35、 100 ml, to be used as distillation receiver fitted with a bored cork stopper continuously vertically notched on the outer surface. 6.8 Filter flask, 500 ml, with vacuum unit. 6.9 Glass wash bottle, 500 ml. 6.10 Cooling bath (see an example on Figure 2), a different cooling bath with the same isolat
36、ion effect can also be used. 6.11 Funnel (in cooling bath), with a diameter of 72 mm and a total length of 200 mm. A jacketed funnel with similar dimensions, connected to the cooling bath, is also allowed. 6.12 Evaporating basin, diameter 80 mm, mark at 15 mm. 6.13 Balance, accurate to 10 mg, readab
37、le to 1 mg. 6.14 Balance, accurate to 2,0 mg, readable to 0,1 mg. 6.15 Laboratory burner (see Figure 3). 6.16 Desiccator 6.17 Porcelain crucible, with a diameter of 80 mm. 6.18 Round filter, with a diameter of 110 mm, for quantitative analysis, transmission: middle close or middle rapid flowing. 6.1
38、9 Timer 6.20 Pincers 7 Sampling Make sure that the laboratory sample is homogeneous and is not contaminated (see EN 1425). Take all necessary safety precautions and ensure that the test sample is representative of the laboratory sample from which it is taken (see EN 58). The laboratory sample shall
39、be taken in accordance with EN 58. The test shall be carried out on two portions each of (25 1) g. Prepare the test sample in accordance with EN 12594. 8 Procedure Melt each test portion in a porcelain crucible for the minimum time necessary to ensure that the sample is completely fluid. Pour (25 1)
40、 g into the distillation flask (6.3) and weigh to the nearest 10 mg (mass mB). Heat the distillation flask with a laboratory burner with a soft flame, approximately 150 mm high, (without a flame cone) that has just ceased to be luminous in such a way that the first distillate drop falls down after 3
41、 min to 4 min. Fit the sheet metal guard ring (see 6.4) loosely on the distillation flask to prevent possible burning of the cork stopper. Ensure that the vapours produced during distillation are being condensed by weighing, to the nearest 10 mg, the Erlenmeyer flask (6.7) into which the lower bent
42、end of the outlet tube projects to its full length DIN EN 12606-1:2015-11 EN 12606-1:2015 (E) 7 (see Figure 2), and immerse this as far as possible into a mixture of finely ground ice and water. The rate of distillation shall remain visible and capable of being checked. Adjust the distillation rate
43、so that (15 5) drops fall from the end of the outlet tube into the distillation receiver every 10 s. Continue heating without adjusting the laboratory burner flame, until the distillation rate slows and no drop falls from the outlet tube over a period of 10 s or after 14 min from the start of distil
44、lation. Continue heating for a further min with a completely non-luminous roaring flame until the flask glows red. Complete the distillation in a maximum of 15 min. Do not transfer the condensate left in the outlet tube after distillation to the distillation receiver. Mix the distillate thoroughly b
45、y gently warming it whilst at the same time, carefully swirling the receiver. Cool the receiver to ambient temperature in a desiccator and weigh the distillate contained in the receiver to the nearest 10 mg (mass mD). Depending on the expected paraffin wax content, add 2 g to 4 g of the distillate i
46、nto a test tube (6.5) and weigh to the nearest 5 mg (mass mE). NOTE 1 If the paraffin wax content cannot be estimated in advance, an initial mass of distillate of approximately 3 g is recommended. Dissolve the weighed mass of distillate in (25 1) ml of ether (5.2) and add (25 1) ml of ethanol (5.3).
47、 Close the test tube with a stopper fitted with a sample temperature transducer (6.2.1) extending down into the liquid and place the test tube in a cooling bath. Cool the bath liquid by adding finely crushed solid carbon dioxide or with a cryostat (see note to 5.7). To ensure the sample temperature
48、is maintained at - 20 C, which will be required later, lower the bath temperature to (- 22 1) C. Transfer (20 1) ml of the washing liquid (5.9) into the test tube fitted with the wash bottle head and cool in the cooling bath (6.10) to (- 20,0 0,5)C, maintain this temperature until filtration is comp
49、lete. Place the round filter (6.18) in the funnel standing in the cooling bath and connect it to the filter flask placed below the cooling bath. Quickly transfer the slurry of crystals produced at (- 20,0 0,5) C to the filter. Rinse the test tube with the cooled washing liquid. Re-adjust the temperature of the washing liquid to (- 20,0 0,5) C and use it again for rinsing the crystal slurry into the filter. Distribute the was
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