RILEM inter-laboratory test on binder rheology test methods DSR and BBR.

Transcription

1 RILEM inter-laboratory test on binder rheology test methods DSR and BBR. Dariusz Sybilski, IBDiM Poland Ann Vanelstrate, CRR Belgium RILEM Technical Committee 182 PEB Performance Testing and Evaluation of Bituminous Materials

2 RILEM TC 182 RR Test RILEM Technical Committee 182 PEB Performance Testing and Evaluation of Bituminous Materials st Round Robin Test on Binder s Rheology nd Round Robin Test on Binder s Rheology

3 Objectives Evaluation of BBR- and DSR-test procedure Determination of repeatability and reproducibility Improvement of test procedures for standardization

4 Binders Pure bitumen SBS low modified binder SBS high modified binder EVA modified binder

5 Testing program BBR DSR Phase I Phase II original binder X X after RTFOT X X after RTFOT and PAV X X

6 Contributing laboratories Laboratory DSR BBR RTFOT PAV A1 Univ. Vienna B1 BRRC B2 Fina Research CH1 EMPA E1 CEDEX E2 REPSOL E3 Centro de Investigacion Elpidio Sanchez Marcos F1 Esso Asphalt Research Laboratories F2 ELF F3 LCPC GB1 SWK Pavement Engineering H1 AKMI (Veszprem) NL1 DWW S1 Royal Institute of Technology S2 NYNAS US1 U.W. Madison

7 Overview of test methods and testing conditions Handling procedure for binders, emphasis on: temperatures for reheating homogenisation sampling Ageing procedures: RTFOT-ageing according to EN PAV-ageing according to AASHTO-standard at 100 C

8 Overview of test methods and testing conditions BBR Testing procedure for calibration and testing: draft ASTM 3 temperatures per binder 3 repetitions per temperature

9 Overview of test methods and testing conditions Dynamic Rheometers measurements of G* and δ temperature: (- 24, -18, -12, -6, 2,) 10, 16, 22, 28, 34, 40, 46, 52, 58, 64, 70, 76 C frequency: 0.1, 1.6, 5, 10, 20, 50 Hz 3 repetitions for one chosen binders Phase I: Phase II: b1 pure bitumen b4 EVA modified bitumen 1 measurement on others Test procedure for DSR (parallel plates): AASHTO TP5

10 Overview of test methods and testing conditions Ring & Ball Softening Point temperature determination according to EN 1427: before RTFOT after RTFOT after RTFOT + PAV

11 BBR-results: principle P Bending Beam Rheometer P 240s time Deflection (mm) 1000 Stiffness (MPa) m(60s) S(60s) Time (s) s Time (s)

12 BBR Precision (after elimination of outliers) Mean values of Coefficient of Variation for all temperatures All binders, original, RFTO or RTFO+PAV aged Repeatability S(60) 2 3% m(60) 1 2% Reproducibility S(60) 5% m(60) 3 5%

13 BBR Determination of SHRP PG (3 measurements per temperature) S (60s) (MPa) m (60s) mean mean stdev mean stdev mean mean stdev mean stdev Temperature ( C) Temperature ( C) Precision on critical temperatures according to SHRP: about 1 C better than one PG-class

14 DSR-results Test geometry L-TC-CY S e d F h Type of loading LINEAR Tension - Compression No. of labs 2 Overview of Dynamic Rheometers L-SH-AN R-SH-PP D p D g T r F h h LINEAR Annular Shear Rotational Shear Parallel Plates 2 15 R-SH-CP T h Rotational Shear Cup & Plate 1 R-TO-PR T L Torsional Shear 1 T

15 Black curve Z b1 original 1E+2 1E+1 1E+0 G*, MPa 1E-1 1E-2 1E-3 1E-4 1E Phase angle, deg Zb1 mean

16 Black curve D b1 original 1E+3 1E+2 1E+1 1E+0 G*, MPa 1E-1 1E-2 1E-3 1E-4 1E Phase angle, deg Db1 mean

17 Dynamic Rheometers Reproducibility Analysis of two sets of results: all types of equipments/geometries DSR-geometries according to recommendations of AASHTO TP5

18 Precision Inter-laboratory precision in AASHTO TP5 Condition Coefficient of Variation (1s %), % Acceptable range of two results (d2s %), % Original G*/sinδ 10,3 29,1 RTFOT G*/sinδ 11,1 31,3 PAV G*sinδ 19,8 56,1

19 Dynamic Rheometers Repeatability and Reproducibility b1 original, G* 1,6Hz Temperature, C CV, % CV in-lab CV inter-lab

20 Dynamic Rheometers Repeatability and Reproducibility b4 RTFO, G* 1,6Hz Temperature, C CV, % CV in-lab CV inter-lab

21 Dynamic Rheometers Repeatability and Reproducibility b4 PAV, G* 1,6Hz Temperature, C CV, % CV in-lab CV inter-lab

22 Dynamic Rheometers Reproducibility %CV for G* b1 all b1 SHRP before elimination of outliers Temperature ( C)

23 Dynamic Rheometers Reproducibility %CV for G* after elimination of outliers b1 all b1 SHRP Temperature ( C)

24 Dynamic Rheometers Reproducibility original G* 1,6Hz %CV SHRP no outlie rs 12 limiting value CV=10,3% 10 Coefficient of Variation, % b1 b2 b3 b Te m pe ra ture, C

25 Dynamic Rheometers Reproducibility RTFO G* 1,6Hz %CV SHRP no outliers 12 limiting value CV=11,1% 10 Coefficient of Variation, % b1 b2 b3 b Te m pe ra ture, C

26 Dynamic Rheometers Reproducibility PAV G* 1,6Hz %CV S HRP no o utlie rs 25 limiting value CV=19,8% 20 Coefficient of Variation, % b1 b2 b3 b Temperature, C

27 Reliability of laboratories Acceptance of results, G, all geometries Acceptance, % original RTFO A BB C D DD E EE G L O Q RS T U V W X Y Z PAV

28 Reliability of laboratories Acceptance of results, PA, all geometries Acceptance, % original RTFO A BB C D DD E EE G L O Q RS T U V W X Y Z PAV

29 Reliability of results for binders Acceptance of results, G, all geometries Acceptance, % original RTFO b1 b2 b3 b4 PAV

30 Reliability of results for binders Acceptance of results, PA, all geometries Acceptance, % original RTFO b1 b2 b3 b4 PAV

31 Comparison of precision of DR and R&B Change of G* per C (%) b1 b4 b2 b Temperature ( C) Binder St. Dev.( C) R&B RILEM Mentioned ( C) (EN1427) EN ,0 0,6 0,7 2 56,6 1,2 1,3 3 85,7 2,7 2,0 4 61,6 2,0 1,3 G* varies % per 1 C Hence: St.Dev. of 10 % corresponds to less than 1 C

32 Average Average Black curve 1,6 Hz SHRP 1,0E+03 1,0E+02 1,0E+01 G*, MPa 1,0E+00 1,0E-01 1,0E-02 1,0E-03 1,0E PA, deg b1 orig b1 RTFO b1 PAV b2 orig b2 RTFO b2 PAV b3 orig b3 RTFO b3 PAV b4 orig b4 RTFO b4 PAV

33 DR Reliability Equipment or geometry other than SHRP: higher risk for incorrect results Higher acceptance of PA than G* results Higher acceptance of results from DSR and SHRP geometries Higher acceptance of results after ageing (more precise recommendations for second phase of test) The same reliability of DSR results for plain and polymer modified binders The precision on G* is comparable or even better than the precision on R&B

34 DR main sources of error Non-linearity of material s behaviour (too high strain) Improper sample geometry: too big plate radius or too thin gap Too high rheometer compliance Deviation of temperature from the target value Improper sample handling and preparation thermal history heterogeneity steric hardening (too long storage of the sample) deficient or excessive sample volume deficient bond between sample and plates Rewriting

35 Conclusions (recommendations for CEN standards) BBR: Reproducibility standard deviation on S(60s): 5 % Reproducibility standard deviation on m(60s): 3-5 % Performance Grade according to SHRP can be determined with a precision of about 1 C (3 measurements per temperature)

36 Conclusions (recommendations for CEN standards) DSR: For EN-standardization purposes, it is recommended to limit rheometers to SHRP-equipment and geometries. Other equipment/geometries can also lead to correct results, but with higher risks For EN-standardization purposes the temperature range should be limited from 10 to 76 C Reproducibility standard deviation on G*: 10% Reproducibility standard deviation on phase angle: 5%

37 Thank you for your attention