DIN EN 14770-2012 Bitumen and bituminous binders - Determination of complex shear modulus and phase angle using a Dynamic Shear Rheometer (DSR) German version EN 14770 2012《沥青和沥青粘合.pdf

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1、August 2012 Translation by DIN-Sprachendienst.English price group 11No 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

2、 75.140; 91.100.50!$hEnglish version EN 14770:2012,English translation of DIN EN 14770:2012-08Bitumen und bitumenhaltige Bindemittel Bestimmung des komplexen Schermoduls und des Phasenwinkels Dynamisches Scherrheometer (DSR);Englische Fassung EN 14770:2012,Englische bersetzung von DIN EN 14770:2012-

3、08Bitumes et liants bitumineux Dtermination du module complexe en cisaillement et de langle de phase Rhomtre cisaillement dynamique (DSR);Version anglaise EN 14770:2012,Traduction anglaise de DIN EN 14770:2012-08SupersedesDIN EN 14770:2006-01www.beuth.deDocument comprises 17 pagesIn case of doubt, t

4、he German-language original shall be considered authoritative.07.12 DIN EN 14770:2012-08 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 responsible German bodies invol

5、ved in its preparation were the Normenausschuss Materialprfung (Materials Testing Standards Committee) and the Normenausschuss Bauwesen (Building and Civil Engineering Standards Committee), Joint Committee NA 062-03-32 GA Bitumen; Prfverfahren und Anforderungen fr die Bindemittel. Amendments This st

6、andard differs from DIN EN 14770:2006-01 as follows: a) NOTE 2 has been added to Subclause 3.3; b) Clause 4 “Principle” has been rendered more precise; c) NOTE 2 has been added to Subclause 5.1; d) Subclause 6.2 “Zero gap setting” has been revised and the previous NOTE 2 has been deleted; e) Clause

7、7 “Sample preparation” has been revised; f) Subclause 7.1 has been restructured and requirements for reheating times have been added; g) a requirement for reheating has been added in Subclause 7.2; h) Subclause 7.3 “Sample manufacturing and storage conditions” has been added; i) Clause 8 “Procedure”

8、 has been revised and NOTE 4 has been added to Subclause 8.3; j) Annex C “Determination of the viscoelastic linear range” has been added. Previous editions DIN EN 14770: 2006-01 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 14770 May 2012 ICS 75.140; 91.100.50 Supersedes EN 14770:2005English

9、Version Bitumen and bituminous binders - Determination of complex shear modulus and phase angle - Dynamic Shear Rheometer (DSR) Bitumes et liants bitumineux - Dtermination du module complexe en cisaillement et de langle de phase - Rhomtre cisaillement dynamique (DSR) Bitumen und bitumenhaltige Binde

10、mittel - Bestimmung des komplexen Schermoduls und des Phasenwinkels - Dynamisches Scherrheometer (DSR) This European Standard was approved by CEN on 7 April 2012. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standar

11、d 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 versions (English,

12、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, Belgium, Bulga

13、ria, 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. EUROPEAN COMMIT

14、TEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management 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 14770:2012: EEN 14770:2012 (E) 2 Conten

15、ts Page Foreword 31 Scope 42 Normative references 43 Terms and definitions .44 Principle 55 Apparatus .56 Preparation of rheometers 67 Sample preparation .78 Procedure .89 Expression of results . 1010 Precision 1111 Test report . 11Annex A (informative) Temperature verification procedure 12Annex B (

16、informative) Determining equilibration time . 13Annex C (informative) Determination of the viscoelastic linear range . 14Bibliography . 15DIN EN 14770:2012-08 EN 14770:2012 (E) 3 Foreword This document (EN 14770:2012) has been prepared by Technical Committee CEN/TC 336 “Bituminous binders”, the secr

17、etariat of which is held by AFNOR/BNP. 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 November 2012, and conflicting national standards shall be withdrawn at the latest by November 2012. Attentio

18、n 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 identifying any or all such patent rights. This document supersedes EN 14770:2005. Compared with EN 14770:2005, the following changes hav

19、e been made: a) Note 2 added to 3.3; b) Principle application clarified in Clause 4; c) Note 2 improved in 5.1; d) Rewording of 6.2 and previous Note 2 deleted; e) 7.1 has been re-structured and requirements for reheating times added; f) requirement for reheating added in 7.2; g) sub-clause 7.3 adde

20、d; h) Clause 8 revised and Note 4 added in 8.3; i) Annex C (informative) added. This European standard is based on IP PM CM-02 1 and XPT 66-065 2. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European S

21、tandard: Austria, 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

22、 the United Kingdom. DIN EN 14770:2012-08 EN 14770:2012 (E) 4 1 Scope This European standard specifies a number of methods using a dynamic shear rheometer (DSR) capable of measuring the rheological properties of bituminous binders. The procedure involves determining the complex shear modulus and pha

23、se angle of binders over a range of test frequencies and test temperatures when tested in oscillatory shear. From the test, the norm of the complex shear modulus, IG*I, and its phase angle, , at a given temperature and frequency can be calculated, as well as the components G, G, J and J of the compl

24、ex shear modulus and of the complex compliance. This method is applicable to un-aged, aged and recovered bituminous binders, cut-backs and bituminous binders stabilised from emulsions. WARNING The use of this European Standard can involve hazardous materials, operations and equipment. This European

25、Standard does not 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 to determine the applicability of regulatory limitations prior to use. 2 Normative referenc

26、es The following documents, 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 1

27、427, Bitumen and bituminous binders Determination of softening point Ring and Ball method EN 12594, Bitumen and bituminous binders Preparation of tests samples 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 norm of the complex shear modulus

28、IG*I ratio of peak stress to the peak strain in harmonic sinusoidal oscillation 3.2 phase angle phase difference between stress and strain in harmonic oscillation 3.3 norm of the complex compliance IJ*I ratio of the peak strain to the peak stress in harmonic sinusoidal oscillation Note 1 to entry: T

29、he real parts of the complex shear modulus IG*I and the complex shear compliance IJ*I are respectively G and J and are associated with the elastic part of material behaviour which represents energy stored during a shear cycle. They are complex shear modulus or complex shear compliance multiplied wit

30、h cosine of phase angle expressed in degrees. The imaginary parts of the complex shear modulus and the complex shear compliance are respectively G and J and are associated with the viscous part of material behaviour which represents energy dissipated during a shear cycle. They are complex shear modu

31、lus or complex shear compliance multiplied with sine of phase angle expressed in degrees. DIN EN 14770:2012-08 EN 14770:2012 (E) 5 3.4 isotherm equation or curve on a graph representing the behaviour of a material at a constant temperature 3.5 isochrone equation or curve on a graph representing the

32、behaviour of a material at a constant frequency 3.6 region of linear viscoelastic behaviour region in which complex dynamic (shear) modulus is independent of (shear) stress or strain 4 Principle A known oscillatory shear stress is applied to the temperature controlled test geometry, in which the bit

33、uminous test specimen is held. The binders strain response to the stress is measured. Alternatively, a known oscillatory shear strain is applied to the test specimen and the resulting shear stress is measured. Except for specific purposes, the test is performed in the region of linear viscoelastic b

34、ehaviour. 5 Apparatus Usual laboratory apparatus and glassware, together with the following: 5.1 Dynamic Shear Rheometer (DSR), with either an integral temperature control system or temperature control attachments, capable of controlling the temperature over a minimum range of 5 C to 85 C with an ac

35、curacy of 0,1 C throughout the test period. The rheometer shall be fitted with parallel plates, with a constant gap across the area of the plates. The temperature control system shall encompass both plates to avoid temperature gradients across the plates. When the test specimen is immersed in liquid

36、 other than water, ensure that the liquid does not affect the properties of the material being analysed. The rheometer shall be able to determine G*, in the range of 1 kPa to 10 MPa ( 2 %) and the phase angle (), in the range 0 to 90 ( 0,1). NOTE 1 For rheometers using an air bearing, and to avoid d

37、amage, the air supply to the bearing should be switched on before the instrument is switched on. When not in use, the spindle should be secured. NOTE 2 When liquid is used to immerse the test specimen, a water/glycol mixture has been found to be suitable. The proportions used depend on how low the t

38、emperature intended for testing is. Rheometers using radio frequency (RF) heating and/or liquid gas cooling or other heating/cooling systems should be used in accordance with the manufacturers instructions. NOTE 3 Where the bottom plate is nominally the same diameter as the top plate, a visual check

39、 should be made to ensure the two plates are vertically aligned. If there is any doubt as to the alignment of the top and bottom plates, the manufacturer, or a qualified technician, should re-align the plate geometry. NOTE 4 Diameters from 8 mm to 25 mm and gap settings from 0,5 mm to 2,0 mm have be

40、en found to be suitable for bituminous binders. In terms of operational ranges, 25 mm plates are generally suitable for stiffnesses in the range 1 kPa to 100 kPa, and 8 mm plates suitable for stiffnesses (|G*|) in the range 100 kPa to 10 MPa. Plates of other diameters can also be used, providing com

41、pliance effects of the instrument do not affect the results (see 6.1, Note 1) and the testing is done in the linear region (see Clause 8). NOTE 5 The fact that the temperature control range is 5 C to 85 C should not be taken to imply that accurate results will necessarily be obtained for all binders

42、 over this range (see 5.1, Note 4 and 6.1, Note 1). Furthermore, temperatures outside this range can also be used, provided the results are not affected by machine compliance. DIN EN 14770:2012-08 EN 14770:2012 (E) 6 5.2 Moulds, sheet materials or vials, for the preparation of the test specimens. Th

43、e moulds or sheet material, where used, shall be of silicone or similar material, which does not adhere to the test specimen. Vials or containers, where used, shall be of an appropriate material and size for the purpose. NOTE The use of grease or other anti-stick products should be avoided because t

44、hey can affect the adherence of the sample to the rheometer plates. 5.3 Oven, ventilated laboratory model, capable of being controlled at temperatures between 50 C and 200 C with an accuracy of 5 C. 6 Preparation of rheometers 6.1 Set up Set up the rheometer in the sequence given in the manufacturer

45、s instructions, including the procedure for the selecting and setting the correct geometry and gap. Select the appropriate oscillation package, if applicable, from the software menu. It is essential that the operational limits of stiffness for the selected geometry are determined. NOTE 1 The selecti

46、on of system geometry may affect the accuracy of results. The manufacturer may have determined the operational limits and this information may be available but, if not, it can be determined by running a test specimen over a range of test temperatures using all the test geometries likely to be used i

47、n practice, and plotting |G*| against either frequency or phase angle (). Where the divergence between the plots for each geometry exceeds 15 %, this is an indication that compliance effects are affecting one or more of the geometries. The chosen geometry(ies) which shows the more rapid fall in |G*|

48、, or the lower phase angle, indicates that its accuracy limit has been reached. Also, for most rheometers generally used for this European Standard, irrespective of the geometry chosen, values of |G*| in excess of 108Pa are likely to be suspect. Software corrections to the stiffness may be acceptable provided appropriate validation is supplied to the operator. NOTE 2 The rheometer and temperature control system should be calibrated at regu