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1、BS EN 1431:2009 ? ? ? ? ? ? ? ? ? ? BS 2000-458:2009 ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? ? Energy Institute, under the brand of IP, publishes and sells all Parts of BS 2000, and all BS EN petroleum test methods that would be Part of BS 2000, both in its annual publication “Standard methods for
2、 analysis and testing of petroleum and related products and British Standard 2000 Parts” and individually. Further information is available from: Energy Institute, 61 New Cavendish Street, London W1G 7AR. Tel: 020 7467 7100. Fax: 020 7255 1472. BS EN 1431:2009 EUROPEAN STANDARD NORME EUROPENNE EUROP
3、ISCHE NORM EN 1431 March 2009 ICS 75.140; 91.100.50Supersedes EN 1431:1999 English Version Bitumen and bituminous binders - Determination of residual binder and oil distillate from bitumen emulsions by distillation Bitumes et liants bitumineux - Dtermination par distillation du liant rsiduel et du d
4、istillat dhuile dans les mulsions de bitume Bitumen und bitumenhaltige Bindemittel - Bestimmung des Destillationsrckstandes und des ldestillates von Bitumenemulsionen mittels Destillation This European Standard was approved by CEN on 17 January 2009. CEN members are bound to comply with the CEN/CENE
5、LEC 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 bibliographical references concerning such national standards may be obtained on application to the CEN Management Centre or to any
6、 CEN member. This European Standard exists in three official versions (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 Management Centre has the same status as the official versions.
7、CEN members are the national standards bodies 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,
8、Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2009 CENAll rights of exploitation in any form and by any means reserved worldwide for CEN national Member
9、s. Ref. No. EN 1431:2009: E BS EN 1431:2009 EN 1431:2009 (E) 2 Contents Page Foreword 3 1 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Principle 5 5 Reagents and materials 5 6 Apparatus .5 7 Sampling .6 8 Procedure .6 9 Calculation 7 10 Expression of results 7 11 Precision .8 12 Tes
10、t report 8 Annex A (normative) Characteristics of thermometer . 12 Bibliography . 13 ? BS EN 1431:2009 EN 1431:2009 (E) 3 Foreword This document (EN 1431:2009) has been prepared by Technical Committee CEN/TC 336 “Bituminous binders”, the secretariat of which is held by AFNOR. This European Standard
11、shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by September 2009, and conflicting national standards shall be withdrawn at the latest by September 2009. Attention is drawn to the possibility that some of the elements of t
12、his document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 1431:1999. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries
13、are bound to implement this European Standard: 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, Sw
14、eden, Switzerland and the United Kingdom. ? BS EN 1431:2009 EN 1431:2009 (E) 4 1 Scope This European Standard specifies a method for the quantitative determination of residual binder and oil distillate in bituminous emulsions. The method can also be used to obtain residue and oil distillate for furt
15、her testing. NOTE The properties of the material recovered in the test are not necessarily the same as those of the original materials from which the emulsion was produced, especially for polymer modified bitumens. WARNING The use of this standard may involve hazardous materials, operations and equi
16、pment. This standard does not purport to address all of the safety problems associated 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 referenc
17、es The following referenced documents are indispensable for the application of this 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
18、 bituminous binders EN 573-3, Aluminium and aluminium alloys - Chemical composition and form of wrought products - Part 3: Chemical composition and form of products EN 1425, Bitumen and bituminous binders Characterization of perceptible properties EN 12594, Bitumen and bituminous binders - Preparati
19、on of test samples ISO 565, Test sieves - Metal wire cloth, perforated plate and electroformed sheet - Nominal sizes of openings 3 Terms and definitions For the purposes of this document, the following definitions apply. 3.1 oil distillate hydrocarbon fraction which is distilled and collected in the
20、 graduated cylinder under conditions specified in this test 3.2 residual binder residue from a bituminous emulsion after distillation of water and oil distillate NOTE Although mentioned as “recovered binder content“ in the EN 13808 specification standard, the residual binder by distillation is being
21、 considered in that case. The EN 13808 specification standard specifies the “recovered binder content“ according to EN 1431, although the appropriate denomination is “residual binder after distillation“. Consequently, it is highly recommended that this correction should be considered when revising t
22、he EN 13808 standard. ? BS EN 1431:2009 EN 1431:2009 (E) 5 4 Principle Water and oil distillate are distilled from the bituminous emulsion, and separated in a graduated cylinder, leaving a residue of residual binder. 5 Reagents and materials 5.1 Cleaning agents,as used conventionally in a laboratory
23、. 5.2 Sodium hydroxide solution, 40 g/l. 6 Apparatus Usual laboratory apparatus and glassware, together with the following: NOTE For details of assembly of the distillation apparatus for the test, see Figure 3. 6.1 Aluminium alloy still (see Figure 1) oriron still, (241+ 5) mm in height by (101 + 1)
24、 mm external diameter with a (3,2 + 0,2) mm thickness wall and a (125 + 5) mm inside diameter ring burner, having holes on the inner circumference and having three appropriate spacers or guide pins, to ensure centring of burner around the still (see Figure 2). Lid (see Figure 1) of suitable dimensio
25、ns to allow two thermometers (6.4) to be inserted through a stopper and an outlet of suitable diameter to enable connection tube to be connected also through a stopper. NOTE All tolerances in sub-clause 6.1 and shown on Figure 1 and Figure 2 are production tolerances for the manufactures of the test
26、 equipment. No calibration/verification concerning these tolerances is valid in Quality Control apart from the thermometer. The ring burner may be replaced by any alternative means of heating provided the same specified temperature and distillation conditions are achieved. In the event of a dispute,
27、 the reference ring burner as heating apparatus shall be used. 6.2 Connection apparatus,consisting of a glass connecting tube with a (12 + 1) mm diameter, tin shield, and standard water cooled glass condenser tube with a metal or borosilicate glass jacket (see Figure 3). 6.3 Graduated cylinder,100 m
28、l, with graduation intervals of 0,5 ml, to comply with ISO 4788. 6.4 Thermometers,two low distillation thermometers, graduated in degrees Celsius, having a range from -2 C to 300 C. Thermometers conforming to the necessary requirements are specified in Annex A. Other temperature measuring devices ma
29、y be used instead of mercury stem thermometers. However, the mercury stem thermometer is the reference device. Therefore any alternative device employed shall be calibrated so as to provide the same readings as would be provided by the mercury stem thermometer, taking into account changed thermal re
30、sponse times compared with the mercury thermometer. For this test method, in which increasing temperatures are read during the test, documented corrections shall be determined in advance and applied to the observed readings. ? BS EN 1431:2009 EN 1431:2009 (E) 6 6.5 Balance, capable of weighing 3 500
31、 g to an accuracy of 0,1 g. 6.6 Bunsen burneror equivalent means of heating. 6.7 Sieve,300 m, complying with R 40/3 of ISO 565. 7 Sampling The laboratory sample shall be sampled in accordance with EN 58, and the test samples shall be prepared in accordance with EN 12594. Ensure that the laboratory s
32、ample is homogeneous and is not contaminated (see EN 1425). 8 Procedure 8.1 Weigh (200,0 + 0,1) g, Am, of the emulsion sample into the still (6.1) which has been previously tared (including lid, clamp, thermometers and gasket, if gasket is used). 8.2 Use a gasket of oiled paper between the still and
33、 its cover, or grind the joint to a tight fit. Securely clamp the cover on the still. 8.3 Insert a thermometer (6.4) through a cork, in each of the two small holes provided in the cover. Adjust the thermometers so that the end of the bulb of one is (6,5 + 1,0) mm from the bottom of the still and the
34、 bulb of the other is (165 + 2) mm from the bottom of the still. 8.4 Place the ring burner (6.1) at (152 + 2) mm from the bottom of the still. Apply heat by lighting this burner and adjusting it to a low flame. Also apply sufficient heat from a Bunsen burner (6.6) to the connecting tube to prevent c
35、ondensation of water in this tube. NOTE The location of the flame of the ring burner at the start of the test is flexible. It can be raised to decrease the risk of foam-over or lowered to the middle of the still for emulsion containing no solvent. A sudden change in temperature reading of the upper
36、thermometer indicates foam on the bulb and heating should be discontinued until foaming ceases. 8.5 Adjust the location of the ring burner from time to time so that a smooth constant distillation occurs throughout the whole procedure. When the reading on the lower thermometer reaches 215 C, lower th
37、e ring burner until the reading on the thermometer is (260 + 5) C. Maintain the temperature at this level for 15 min. Complete the total distillation in (60 15) min from the first application of heat. If the residual binder as mass percentage is not to be determined (see Clause 9), i.e. distillation
38、 has been performed only to get residual binder for further testing, cooling and weighing (8.6 and 8.7) are not necessary. Proceed directly to 8.8. 8.6 At the end of the heating period, allow the still and accessories to cool down before weighing. Weigh the still and accessories and determine the ma
39、ss of residue after distillation, Bm. Reheat the still containing the sample up to (260 + 5) C for further processing of the residue (see 8.8) 8.7 Record the volume, D, of oil distillate in the graduated cylinder (6.3) to the nearest 0,5 ml. NOTE To improve the separation of water and oil, 5 ml of s
40、odium hydroxide solution (5.2) may be added to distillates from cationic emulsions. ? BS EN 1431:2009 EN 1431:2009 (E) 7 8.8 Remove the cover from the still. Stir the residue, and pour it immediately through a 300 m sieve (6.7) heated at the same temperature prior to use. Transfer sufficient quantit
41、ies of the residue into suitable moulds and containers for carrying out any required further tests. Handle or condition moulds and containers for examination of the residue as described in EN 12594 and proceed as required by the appropriate EN test method from the steps that follow the pouring stage
42、. Retain the oil distillate for identification if required. 9 Calculation Calculate the residual binder after distillation, r, as mass percentage, using the following equation: r B A m m x 100=(1) where Amis the mass of emulsion sample, in grams (see 8.1); Bmis the mass of the residue after distilla
43、tion, in grams (see 8.6). Calculate the oil distillate (o), as a volume percentage, using the following equation: 100 m = A D o (2) where D is the volume of oil distillate, in millilitres (see 8.7). is the density of the emulsion, in g/ml. NOTE The density of the emulsion, ,is assumed to be 1 000 kg
44、/m (1 g/ml) at 15 C. 10 Expression of results Express the residual binder (see Note in 3.2) as a mass percentage to the nearest 1 %. Express the oil distillate as a volume percentage to the nearest 0,1 %. The binder content of the emulsion determined by the distillation method described in this meth
45、od shall be defined as the mass percentage of the residual binder plus the mass percentage of oil distillate. NOTE Based on the volume percentage of oil distillate, the mass percentage of oil distillate m, may be determined on bulk quantities of flux following the determination of density, in accord
46、ance with EN ISO 3838. If the density cannot be determined in this way, a value of 0,850 may be assumed. ? BS EN 1431:2009 EN 1431:2009 (E) 8 11 Precision 11.1 Repeatability The difference between two successive test results, obtained by the same operator with the same apparatus under constant operating conditions on identical test material would in the long run, in the normal and correct operations of