Warm mix study with the use of wax modified asphalt binders Geoffrey M. Rowe Gaylon L. Baumgardner Gerald Reinke John A. D'Angelo David Anderson Binder ETG Meeting Irvine, CA Wednesday, February 25, 2009
Objectives To investigate the effect on rheology and performance of various warm mix additives with various was additives
Materials tested 9 - Waxes 0 Lion Oil PG 64-22 1 Romanta Normal Montan 2 Romanta Asphaltan A 3 Romanta Asphaltan B 4 Licomont BS 100 5 Sasobit 6 Luxco Pitch # 2 7 Alphamin GHP 8 Strohmeyer and Arpe Montan LGE 9 Astra Wax 3816D Microcrystalline
Test program Binder M320 Table 1 and 2 Binder master curves BBR and DSR BBR tests at different aging conditions (0, 2, 4, 8, 16 and 32 days) MSCR Mixture Mix BBR tests 2 temperatures for limited mastercurves Repeated creep tests Fatigue monotonic tests and repeated load Master curves
Mix stiffness in BBR Tested BBR beams at varying ageing Analysis extended to use 1000 second data Removed early part of test data to avoid effects of non-instantaneous startup
Binder test data
PG grading AASHTO M320
Viscosity changes 0.46 0.44 0.42 0.40 0.38 0.36 0.34 0.32 0.30 40 35 30 25 20 15 10 5 0 Alphamin GHP Strohmeyer and Arpe Montan LGE Astra Wax 3816D Microcrystalline Lion Oil PG 64-22 Romanta Normal Montan Romanta Asphaltan A Romanta Asphaltan B Licomont BS 100 Sasobit Luxco Pitch # 2 Viscosity at 135 o C, Pa.s Viscosity Reduction, %
Binder 0 day tests RHEOLOGY ANALYIS in Abatech RHEA Software RHEOLOGY OBSERVATIONS 6 (Luxco Pitch # 2) has lower G* mastercurve Significant difference in G* at lower end of frequency range δ with various binders show some type of network at low frequencies, more significant in 2 (Romanta Asphaltan A), 3 (Romanta Asphaltan B), 4 (Licomont BS 100), 5 (Sasobit) and 7 (Alphamin GHP) Judging from δ (at low temp/high freq.) 6 (Luxco Pitch # 2) appears to have best relaxation properties 9 (Astra Wax 3816D Microcrystalline) has worse relaxation properties
Master curve E*, T ref = 25 o C G*, Pa 1.0E+09 1.0E+08 1.0E+07 1.0E+06 1.0E+05 1.0E+04 G* (0) G* (1) G* (2) G* (3) G* (4) G* (5) G* (6) G* (7) G* (8) G* (9) LOG-LOG SCALE 1.0E+03 1.0E+02 1.0E+01 1.0E+00 1.0E-06 1.0E-05 1.0E-04 1.0E-03 1.0E-02 1.0E-01 1.0E+00 1.0E+01 1.0E+02 1.0E+03 1.0E+04 1.0E+05 1.0E+06 1.0E+07 Frequency, rads/sec
Master curve E*, T ref = 25 o C G*, Pa 3.5E+08 3.0E+08 2.5E+08 2.0E+08 1.5E+08 G* (0) G* (1) G* (2) G* (3) G* (4) G* (5) G* (6) G* (7) G* (8) G* (9) 1.0E+08 LOG-LINEAR SCALE 5.0E+07 0.0E+00 1.0E-06 1.0E-05 1.0E-04 1.0E-03 1.0E-02 1.0E-01 1.0E+00 1.0E+01 1.0E+02 1.0E+03 1.0E+04 1.0E+05 1.0E+06 1.0E+07 Frequency, rads/sec
Binder 0 0 days
Binder 1 0 days
Binder 2 0 days
Binder 3 0 days
Binder 4 0 days
Binder 5 0 days
Binder 6 0 days
Binder 7 0 days
Binder 8 0 days
Binder 9 0 days
Jnr Tests conducted at three temperatures 58, 64, 70 o C Jnr evaluated at 3.2 kpa and 4 (1/kPa) Elastic recovery v. high for some products at low stress levels Certain products are more stress dependent that conventional binders
2 % Recovery 58 to 64C % recovery MSCR 100 90 80 70 60 50 40 30 20 10 0 10 3.2 kpa 3.2 kpa 3.2 kpa 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 5 5.5 Jnr 1/kPa 2 58C 2 64C 2 70C
Recovery near grade temp 100 % Recovery 90 80 70 60 50 40 30 7 4 5 0 64C 1 64C 2 70C 3 64C 4 70C 5 70C 6 58C 7 70C 8 58C 9 58C 20 10 0 2 6 10 0 1 2 3 4 5 6 7 8 9 10 11 Jnr 1/kPa
Jnr at 64 o C 12 0 1 2 3 4 5 6 7 8 9 10 8 Jnr, 1/kPa 6 4 2 0 0.01 0.1 1 10 100 Stress, kpa
Jnr near grade temperature 12 Jnr 1/kPa 10 8 6 0 64C 1 64C 2 70C 3 64C 4 70C 5 70C 6 58C 7 70C 8 58C 9 58C 4 2 0 0.01 0.1 1 10 100 Stress kpa
Jnr versus % recovery 100 90 80 % recovery 70 60 50 40 30 Elastic 20 10 0 Non-Elastic 0 2 4 6 8 10 12 14 16 18 20 Jnr, 1/kPa
PG grades M320 Table 3 PG Range G*/sind - TANK G*/sind - RTFOT G*sind - PAV BBR S BBR m-value PG Range (Jnr) Jnr 1/kPa @ 3200 Pa 90 100 80 70 60 50 40 30 20 10 0-10 -20-30 Lion Oil PG 64-22 Romanta Normal Montan Romanta Asphaltan A Romanta Asphaltan B Licomont BS 100 Sasobit Luxco Pitch # 2 Alphamin GHP Strohmeyer and Arpe Montan LGE Astra Wax 3816D Microcrystalline
Difference in performance Binders grade different in Jnr evaluation Can be as much ½ PG grade Early products that show network 2 effected from 5 2 (Romanta Asphaltan A) 3 (Romanta Asphaltan B) 4 (Licomont BS 100) 5 (Sasobit) 7 (Alphamin GHP) Suggests importance of Jnr evaluation
Aged tests - binder
PG64-22 aging to 32 days 10000-18 o C Day 0 Day 2 Day 4 Day 8 Day 16 Day 32 Stiffness, MPa 1000 100 1 10 100 1000 Time, seconds
Binder BBR S(t) at -12 o C 500 Binder BBR Stiffness, -12 o C, t = 60 seconds 450 400 Stiffness, MPa 350 300 250 200 150 0 5 10 15 20 25 30 35 Aging Time, days 0 Lion Oil PG 64-22 1 Romanta Normal Montan 2 Romanta Asphaltan A 3 Romanta Asphaltan B 4 Licomont BS 100 5 Sasobit 6 Luxco Pitch # 2 7 Alphamin GHP 8 Strohmeyer and Arpe Montan LGE 9 Astra Wax 3816D Microcrystalline
Binder BBR S(t) at -18 o C 900 Binder BBR Stiffness, -18 o C, t = 60 seconds 800 Stiffness, MPa 700 600 500 400 300 0 5 10 15 20 25 30 35 Aging Time, days 0 Lion Oil PG 64-22 1 Romanta Normal Montan 2 Romanta Asphaltan A 3 Romanta Asphaltan B 4 Licomont BS 100 5 Sasobit 6 Luxco Pitch # 2 7 Alphamin GHP 8 Strohmeyer and Arpe Montan LGE 9 Astra Wax 3816D Microcrystalline
BBR data Aging data showed that the -18 o C gave significantly more variability when compared to the -12 o C data
Mix test data
Mix BBR Data Data processed to produce equallog scale representation with approximate linear double of scale Several cases exist which colder temperature is less stiff than matching warm temperature data
Removal of early BBR data Data before 8- seconds is removed from analysis in similar manner to binder BBR data Shows fitted (polynomial) approach versus direct calculation Data before t=8 seconds is less reliable Stiffness, MPa (Direct) 25,000 20,000 15,000 10,000 5,000 5000 10000 15000 20000 25000 Stiffness, MPa (fitted) Data point corresponding to 8 seconds
0-0
0-16
0-32
5-0
5-16
Material 5 - Day 16 100,000 16-91-5-1-12 16-91-5-1-18 16-91-5-2-12 16-91-5-2-18 16-91-5-3-12 16-91-5-3-18-18 -12 S(t), MPa 10,000 1,000 0.1 1 10 100 1000 t, seconds
Re-tests of Mix Beams Testing of beams before and after annealing Annealing conducted at 64 o C overnight 64 o C chosen since it represents day at likely high-pavement temperature
1 - PG64-22 - retests 0-3-RR 0-1 & 2-RRA 0-1-RR 0-3-RRA
5 - Sasobit -retests 5-2 & 3-RR 5-3-RRA 5-1-RRA
9 - Astra Wax 9-3-RRA 9-3-RR
Results from retesting In all cases healing overnight increased the stiffness of the mastercurve Most significantly it resulted in the BBR stiffness of the -18 o C isotherm being greater than the -12 o C isotherm as expected! The healing is more significant for the -18 o C isotherm
Repeated creep torsion bar Tests at two stress levels 34 and 68 kpa Temperature = 64 o C 5 replicates used results of middle 3 Analysis of various parameters
Repeated load tests Normalized Parameter 1 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 Strain (normalized) Slope Cycles/Strain Flow Number Flow Number (mod.) Steady creep area 0 500 1000 1500 2000 2500 3000 3500 Time, seconds Concept used in early 1990 s with cyclic deformation tests Based on same concept as used for fatigue analysis Very ease to use to limit test time stop test at say 5% less than max
Jnr Grade vs. Repeated Creep 700 Flow Number (modified) Repeated Creep Performance 600 1/slope y = 9E-07x 4.6648 min dy/dx R 2 = 0.7589 500 400 300 y = 6E-08x 5.1932 R 2 = 0.7633 200 100 y = 6E-09x 5.4748 R 2 = 0.8031 0 52 58 64 70 76 82 High PG Grade using Jnr, o C
Jnr at 64 o C vs. Repeated Creep 700 Repeated Creep Performance 600 500 400 300 200 100 Flow Number (modified) 1/slope min dy/dx y = 467.69x -0.5795 R 2 = 0.743 y = 302.97x -0.6394 R 2 = 0.734 0 y = 112.64x -0.6689 R 2 = 0.7603 0 1 2 3 4 5 6 7 8 9 10 Jnr, 64 o C (3.2 kpa)
Fatigue Work conducted by MTE Services, Inc Monotonic loading test Sand cylinders repeated loading
Monotonic tests 1.60E+09 1.40E+09 AREA UNDER MONOTONIC TEST CURVE AT PEAK VALUE 3% Wax Blends 1.20E+09 1.00E+09 8.00E+08 6.00E+08 4.00E+08 2.00E+08 0.00E+00 RELATIVE AREA VALUE control Montan Asphaltan A Asphaltan B Licomont BS 100 Sasobit Luxco Pitch Alphamin GHP Montan LGE Astra 3816
1.60E+09 1.40E+09 1.20E+09 1.00E+09 8.00E+08 6.00E+08 4.00E+08 2.00E+08 0.00E+00 RELATIVE AREA VALUE control Montan Asphaltan A Asphaltan B Licomont BS 100 Sasobit Luxco Pitch Alphamin GHP Montan LGE Astra 3816 Monotonic tests AREA UNDER MONOTONIC TEST CURVE AT PEAK VALUE AREA 1% BLENDS ADDED SOME 1% Wax Blends
Sand Cylinder Fatigue SECONDS TO FAILURE AT 10 HZ FREQUENCY 1E+06 1E+05 1E+04 TESTS AT 600, 1000 AND 1800 MICROSTRAIN Generally all modifiers give poorer performance but difference is very small compared to other materials and typical noise in fatigue sets 1000 500.0 1000.0 MICROSTRAIN 91-0 control 91-1 Original Montan 91-2 Asphaltan A 91-3 Asphaltan B 91-4 Licomont 91-6 Luxco Pitch 91-7 Alphamin GHP 91-8 Montan LGE 91-9 Astra 3816 91-5 SASOBIT
Master curves on sand-mix
Merged MasterCurve Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 #1 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 10 6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 Ξ [rad/s]
Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 G* Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 ω [rad/s]
Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 G* Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 Average MasterCurves Paragon Wax Study, 91-1-07, Wax #1, 6 7% AV, T-F, 20 to 60 0 10 6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 ω [rad/s]
Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 G* Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 Average MasterCurves Paragon Wax Study, 91-1-07, Wax #1, 6 7% AV, T-F, 20 to 60 0 Average Merged MasterCurves Paragon Wax Study, 91-2-10, Wax #2, 7 1% AV, T-F, -30 to 60 10 6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 ω [rad/s]
Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 10 6 G* Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 Average MasterCurves Paragon Wax Study, 91-1-07, Wax #1, 6 7% AV, T-F, 20 to 60 0 Average Merged MasterCurves Paragon Wax Study, 91-2-10, Wax #2, 7 1% AV, T-F, -30 to 60 Average MasterCurve Paragon Wax Study, 91-3-14, Wax #3, 6 6% AV, T-F, -30 to 60 0 10-6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 ω [rad/s]
Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 10 6 G* Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 Average MasterCurves Paragon Wax Study, 91-1-07, Wax #1, 6 7% AV, T-F, 20 to 60 0 Average Merged MasterCurves Paragon Wax Study, 91-2-10, Wax #2, 7 1% AV, T-F, -30 to 60 Average MasterCurve Paragon Wax Study, 91-3-14, Wax #3, 6 6% AV, T-F, -30 to 60 0 Average Merged MasterCurves Paragon Wax Study, 91-4-17, Wax #4, 6 7% AV, -30 to 60 0 10-6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 ω [rad/s]
Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 G* Average MasterCurves, 91-0-01, Control, 7 1% AV, -30 to 60 0 Average MasterCurves, 91-1-07, Wax #1, 6 7% AV, T-F, 20 to 60 0 Average MasterCurves, 91-2-10, Wax #2, 7 1% AV, T-F, -30 to 60 Average MasterCurve 91-3-14, Wax #3, 6 6% AV, T-F, -30 to 60 0 Average MasterCurves, 91-4-17, Wax #4, 6 7% AV, -30 to 60 0 Average MasterCurves, 91-05-22, Wax #5, 7 1% AV, T-F, -30 to 60 10 6 10-6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 ω [rad/s]
Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 G* Average MasterCurves, 91-0-01, Control, 7 1% AV, -30 to 60 0 Average MasterCurves, 91-1-07, Wax #1, 6 7% AV, T-F, 20 to 60 0 Average MasterCurves, 91-2-10, Wax #2, 7 1% AV, T-F, -30 to 60 Average MasterCurve 91-3-14, Wax #3, 6 6% AV, T-F, -30 to 60 0 Average MasterCurves, 91-4-17, Wax #4, 6 7% AV, -30 to 60 0 Average MasterCurves, 91-05-22, Wax #5, 7 1% AV, T-F, -30 to 60 Average MasterCurves, 91-6-25, Wax #6, 7 1% AV, T-F, -30 to 60 0 10 6 10-6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 ω [rad/s]
Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 G* Average MasterCurves, 91-0-01, Control, 7 1% AV, -30 to 60 0 Average MasterCurves, 91-1-07, Wax #1, 6 7% AV, T-F, 20 to 60 0 Average MasterCurves, 91-2-10, Wax #2, 7 1% AV, T-F, -30 to 60 Average MasterCurve 91-3-14, Wax #3, 6 6% AV, T-F, -30 to 60 0 Average MasterCurves, 91-4-17, Wax #4, 6 7% AV, -30 to 60 0 Average MasterCurves, 91-05-22, Wax #5, 7 1% AV, T-F, -30 to 60 Average MasterCurves, 91-6-25, Wax #6, 7 1% AV, T-F, -30 to 60 0 Average MasterCurves, 91-07-29, Wax #7, 7% AV, -30 to 60 10 6 10-6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 ω [rad/s]
Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 10 6 G* Average MasterCurves, 91-0-01, Control, 7 1% AV, -30 to 60 0 Average MasterCurves, 91-1-07, Wax #1, 6 7% AV, T-F, 20 to 60 0 Average MasterCurves, 91-2-10, Wax #2, 7 1% AV, T-F, -30 to 60 Average MasterCurve 91-3-14, Wax #3, 6 6% AV, T-F, -30 to 60 0 Average MasterCurves, 91-4-17, Wax #4, 6 7% AV, -30 to 60 0 Average MasterCurves, 91-05-22, Wax #5, 7 1% AV, T-F, -30 to 60 Average MasterCurves, 91-6-25, Wax #6, 7 1% AV, T-F, -30 to 60 0 Average MasterCurves, 91-07-29, Wax #7, 7% AV, -30 to 60 Average MasterCurves 91-08-33, Wax #8, 6,9% AV, -30 to 60 10-6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 ω [rad/s]
Average Merged MasterCurves Paragon Wax Study, 91-0-01, Control, 7 1% AV, -30 to 60 0 10 11 10 10 G* ( ) [Pa] 10 9 10 8 10 7 10 6 G* Average MasterCurves, 91-0-01, Control, 7 1% AV, -30 to 60 0 Average MasterCurves, 91-1-07, Wax #1, 6 7% AV, T-F, 20 to 60 0 Average MasterCurves, 91-2-10, Wax #2, 7 1% AV, T-F, -30 to 60 Average MasterCurve 91-3-14, Wax #3, 6 6% AV, T-F, -30 to 60 0 Average MasterCurves, 91-4-17, Wax #4, 6 7% AV, -30 to 60 0 Average MasterCurves, 91-05-22, Wax #5, 7 1% AV, T-F, -30 to 60 Average MasterCurves, 91-6-25, Wax #6, 7 1% AV, T-F, -30 to 60 0 Average MasterCurves, 91-07-29, Wax #7, 7% AV, -30 to 60 Average MasterCurves 91-08-33, Wax #8, 6,9% AV, -30 to 60 Average MasterCurves 91-09-38, Wax #9, 7 1% AV, T-F, -30 to 60 0 10-6 10-5 10-4 10-3 10-2 10-1 10 0 10 1 10 2 10 3 10 4 10 5 10 6 10 7 10 8 10 9 10 10 10 11 ω [rad/s]
Summary Binder tests Significant differences in PG grades with different modifiers All had some loss of performance at low end of specification Master curves show different structures in binder note low strain level Jnr results show that binder is stress sensitive Wax products generally vary more with stress level Have apparently good behavior at low stress levels As stress level increases performance drops The wax materials are a non-elastic modifier Note δ can confuse the analysis such as used in some specifications Aging of BBR binder beams over extended time shows significant change in properties Data at -12C was more in line with that expected Data at -18C appears to be confounded
Summary mix tests BBR Avoid using early part of isotherm Issues with -18C data after extended aging Some damage/healing evident in data Annealing at 64C showed that rankings could be restored to that expected -18C is poorer than -12C data Repeated creep Data lines up with Jnr results Some suggestions for data analysis Fatigue Monotonic tests show difference in performance Preliminary 1% and 3% wax show some different results Repeated loading shows again significant differences all waxes generally give lower performance but difference is small Master curves Differences evident in G* master curves Should be able to look at these combined with BBR master curves
What to do More work with 1% wax content Some additional analysis of data Maybe combine G* and S(t) master curves for mix to look at trends do they match binder? DTT with notched specimens Develop report
Questions, comments and discussion please!!?? Del Mar Shores Beach Park, CA 2009/2/22