BS 2000-536-2005 Methods of test for petroleum and its products Bitumen and bituminous binders — Determination of complex shear modulus and phase angle — Dynamic Shear Rheometer (D.pdf

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1、BRITISH STANDARDBS 2000-536:2005 BS EN 14770:2005Methods of test for petroleum and its products. Bitumen and bituminous binders Determination of complex shear modulus and phase angle Dynamic Shear Rheometer (DSR)(Identical with IP 536:2005)The European Standard EN 14770:2005 has the status of a Brit

2、ish StandardICS 75.140; 91.100.50g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58Licensed Copy: Wang Bin, na, Tue Apr 18 02:33:26 BST 2006, Uncontro

3、lled Copy, (c) BSIBS EN 14770:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 10 January 2006 BSI 10 January 2006ISBN 0 580 46851 8National forewordThis British Standard is the official English language version of EN 14770:2005. The UK pa

4、rticipation in its preparation was entrusted to Technical Committee PTI/13, Petroleum testing and terminology, which has the responsibility to:A list of organizations represented on this committee can be obtained on request to its secretary.Energy Institute, under the brand of IP publishes and sells

5、 all parts of BS 2000, and all BS EN petroleum test methods that would be part of BS 2000, both in its natural publication Standard methods for analysis and testing of petroleum and related products and British Standard 2000 parts and individually.Further information is available from:Energy Institu

6、te, 61 New Cavendish Street, London W1G 7AR. Tel: 020 7467 7100. Fax: 020 7255 1472.Cross-referencesThe British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspo

7、ndence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application.Compliance with a British Standard does not of it

8、self confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep UK interests informed; monitor related international and European developments and pro

9、mulgate them in the UK.Summary of pagesThis document comprises a front cover, an inside front cover, the EN title page, pages 2 to 13 and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date Comm

10、entsLicensed Copy: Wang Bin, na, Tue Apr 18 02:33:26 BST 2006, Uncontrolled Copy, (c) BSIEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14770October 2005ICS 75.140; 91.100.50English VersionBitumen and bituminous binders - Determination of complexshear modulus and phase angle - Dynamic Shear Rheom

11、eter(DSR)Bitumes et liants bitumineux - Dtermination du modulecomplexe en cisaillement et de langle de phase -Rhomtre cisaillement dynamique (DSR)Bitumen und bitumenhaltige Bindemittel - Bestimmung deskomplexen Schermoduls und des Phasenwinkels -Dynamisches Scherrheometer (DSR)This European Standard

12、 was approved by CEN on 26 August 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such n

13、ationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and no

14、tified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherla

15、nds, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and

16、 by any means reservedworldwide for CEN national Members.Ref. No. EN 14770:2005: ELicensed Copy: Wang Bin, na, Tue Apr 18 02:33:26 BST 2006, Uncontrolled Copy, (c) BSIEN 14770:2005 (E) 2 Contents Page Foreword 3 1 Scope .4 2 Normative references .4 3 Terms and definitions.4 4 Principle.5 5 Apparatus

17、 5 6 Preparation of rheometers .6 7 Sample preparation.7 8 Procedure 7 9 Expression of results9 10 Precision9 11 Test report .10 Annex A (informative) Temperature verification procedure11 Annex B (informative) Determining equilibration time 12 Bibliography.13 Licensed Copy: Wang Bin, na, Tue Apr 18

18、02:33:26 BST 2006, Uncontrolled Copy, (c) BSIEN 14770:2005 (E) 3 Foreword This European Standard (EN 14770:2005) 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 standar

19、d, either by publication of an identical text or by endorsement, at the latest by April 2006, and conflicting national standards shall be withdrawn at the latest by April 2006. This European standard is based on IP PM CM-02 1 and XPT 66-065 2. According to the CEN/CENELEC Internal Regulations, the n

20、ational standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,

21、 Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Licensed Copy: Wang Bin, na, Tue Apr 18 02:33:26 BST 2006, Uncontrolled Copy, (c) BSIEN 14770:2005 (E) 4 1 Scope This European Standard specifies a number of methods using a dynamic shear rheometer (DSR) capable of measuri

22、ng the rheological properties of bituminous binders. The procedure involves determining the complex shear modulus and phase 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 ph

23、ase angle, , at a given temperature and frequency can be calculated, as well as the components G, G, J and J of the complex shear modulus and of the complex compliance. This method is applicable to unaged, aged and recovered bituminous binders, cut-back or fluxed bituminous binders stabilised from e

24、mulsions. WARNING The use of this standard can involve hazardous materials, operations and equipment. 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 health and safety practic

25、es and determine the applicability of regulatory limitations prior to use. 2 Normative references 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 referen

26、ced document (including any amendments) applies. EN 1427, Bitumen and bituminous binders Determination of softening point Ring and Ball method. EN 12594, Bitumen and bituminous binders Preparation of test samples. 3 Terms and definitions For the purposes of this European Standard, the following term

27、s and definitions apply. 3.1 norm of the complex shear modulus 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 sinusoidal oscillation 3.3 norm of the complex shear compliance IJ*I ratio of the peak

28、 strain to the peak stress in harmonic sinusoidal oscillation NOTE The 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 the material behaviour. The imaginary parts of the complex shear modulus and

29、the complex shear compliance are respectively G and J and are associated with the viscous part of the material behaviour. The tangent of the phase angle represents the ratio of its viscous component over its elastic component (e.g. tan equals G”/G or J”/J). Licensed Copy: Wang Bin, na, Tue Apr 18 02

30、:33:26 BST 2006, Uncontrolled Copy, (c) BSIEN 14770:2005 (E) 5 3.4 isotherm equation or curve on a graph representing the behaviour of a material at a constant temperature 3.5 isochron equation or curve on a graph representing the behaviour of a material at a constant frequency 3.6 region of linear

31、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 is held the bituminous test specimen. The binders strain response to the str

32、ess is measured. Alternatively, a known oscillatory shear strain is applied to the test specimen and the resulting shear stress is measured. 5 Apparatus Usual laboratory apparatus and glassware, together with the following: 5.1 Dynamic Shear Rheometer (DSR), with either an integral temperature contr

33、ol system or temperature control attachments, capable of controlling the temperature over a minimum range of 5 C to 85 C with an accuracy 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 contro

34、l system shall encompass both plates, to avoid temperature gradients across the plates. Where the test specimen is immersed in liquid 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

35、 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 damage, 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

36、used to immerse the test specimen, a water/glycol mixture has been found to be suitable. The proportions used depend on how low a temperature it is intended to test. Rheometers using radio frequency (RF) heating and/or liquid gas cooling should be used in accordance with the manufacturers instructio

37、ns. NOTE 3 Where the bottom plate is nominally the same diameter as the top plate, then a visual check 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, then the manufacturer, or a qualified technician, should re-a

38、lign the plate geometry. NOTE 4 For information, diameters from 8 mm to 25 mm and gap settings from 0,5 mm to 2,0 mm have been 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 plate

39、s suitable for stiffnesses (|G*|) in the range 100 kPa to 10 MPa. Plates of other diameters can also be used, providing compliance effects of the instrument are not affecting the results (see 6.1, Note 1) and the testing is done in the linear region, see 8. NOTE 5 The fact that the temperature contr

40、ol range is 5 C to 85 C should not be taken to imply that accurate results will necessarily be obtained for all binders over this range (see 5.1, Note 4 and 6.1, Note 1). Also temperatures outside this range can be used provided results are not affected by machine compliance. Licensed Copy: Wang Bin

41、, na, Tue Apr 18 02:33:26 BST 2006, Uncontrolled Copy, (c) BSIEN 14770:2005 (E) 6 5.2 Moulds, sheet materials or vials, for the preparation of the test specimens. The moulds or sheet material, where used, shall be of silicone or similar material, which does not adhere to the test specimen. Vials or

42、containers, where used, shall be of an appropriate material and size for the purpose. 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 i

43、n the manufacturers 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.

44、NOTE 1 The selection 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 l

45、ikely to be used in 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

46、rapid fall in |G*|, or the lower phase angle, indicates that its accuracy limit has been reached. Also, for most rheometers generally used for this standard, irrespective of geometry chosen, values of |G*| in excess of 108Pa are likely to be suspect. Software corrections to the stiffness may be acce

47、ptable provided appropriate validation is supplied to the operator. NOTE 2 The rheometer and temperature control system should be calibrated at regular intervals in accordance with the quality assurance procedure of the laboratory. A suitable method is that the rheometer and temperature control syst

48、em should be calibrated by a means traceable to a national standard. Also, it is adviseable to verify the accuracy of the temperature control system by means of a certified temperature measuring device at regular intervals. Also note that external devices read the accurate temperature value only if

49、they are calibrated correctly. A temperature verification procedure is described in Annex A. NOTE 3 The temperature in the test sample may differ from the temperature read by the device if insufficient equilibration time is used. A procedure for determining equilibration time is described in Annex B. 6.2 Gap setting Set the gap between the plates prior to loading the test specimen, with both plates at nominally the same temperature. NOTE 1 Gap settings within the range 0,5 mm to 2,0 mm have been found to be suitabl