DSR-PAV Test Improvement

2Q17 Status Update

AI TAC TF members:
Pavel Kriz (Imperial Oil/ExxonMobil)
Gerry Reinke (Mathy)
Mike Anderson (Asphalt Institute)
Wes Cooper (Asphalt Institute)
Dave Anderson (Consultant)
Expert Task Group Meeting, Ames IA
May 3, 2017
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 Case for Action: DSR-PAV Is Too
Variable
6163 kPa One Sample Multiple Samples
Gauge R&R
SQC Data Production Data
5600 UCL=5507 60% 57%
Reproducibility, 40.2%

50%
DSR-PAV, kPa

4800
_ 40% Unacceptable
X=4349

4000 30%
20% Acceptable
3200 LCL=3190
w/limits
10%
Acceptable
1 30 60 90 1 30 60 0%
Gauge
2728 kPa R&R
Observation

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 Connect from September ETG
• Initial study presented - indicated test strain & plate size as likely
contributors to DSR-PAV variability
• TF formed within AI TAC
• Labs volunteered to participate in RR to collect data for the study

17 labs participating in round robin

Imperial Oil/ExxonMobil Asphalt Institute MTO
Holly Frontier Corp. PRI Asphalt Technologies Delaware DOT
Flint Hills Resources (3 labs) Road Science Washington State DOT
Paragon Technical Services Kraton Polymers
Jebro Pike Industries Inc.
MTE Services Alon Asphalt

Thank you all for volunteering!!!

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 Development since the last ETG
1. TF expanded scope  DSR conditioning time
1. Stage 1 to determine appropriate conditioning time
2. Stage 2 to test effect of strain & plate size on variability
2. Asphalt Institute developed & distributed 2 PAV asphalt samples (NC-B, NC-D)
3. Test protocol developed & shared
– Included a diverse set of DSRs & T-control systems to ensure broad applicability
– Standardized sample preparation & loading
– Developed excel sheet to collect and analyze data for stage 1
– 2 PAV aged asphalts & Cannon standard tested

Instruments in round robin

Manufacturer DSR Type Count
Anton Paar 101, 102, SmartPave 4
Thermal Analysis AR500 1
AR2000, AR2000ex 1
DHR-2 2
ARES (rheometrics) 1
Malvern (Bohlin) DSR II 1
CVO-100 2
Kinexus 2 4
 Test Protocol for Stage I
Test Protocol Highlights Test Setups Used in DoE
• Samples aliquoted to small Sample Plate size, mm Temperature, °C

tins by AI & distributed Cannon 8 13

Cannon 25 13
• Standardized approach on Cannon 8 25
sample heating & loading Cannon 25 25
• Cooling from 46 °C to target NC-B 8 13
temperature left to NC-B 25 13

instrument control system NC-B 8 19

NC-B 25 19
• Dynamic data collected in NC-D 8 19
30 s interval during cooling NC-D 25 19
& isothermal portion for 30 NC-D 8 25
mins in total NC-D 25 25

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 Stage I – Finding Conditioning Time
Objective: Verify that current 10 min time is appropriate across variety of systems
Analysis: Complex approach – Dave Anderson is going to explain later

Isothermal hardening
Modulus

Cannon standard

Temperature
Sensor T

Conditioning
Time (?)

time=0, time=test
T within 0.1°C
Time
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 Initial Stage 1
Data Analysis
(8* out of 17 labs)
*Labs 13 & 15 (same instrument type) excluded from analysis, >3 sigma.
 Cooling to Temp. is Relatively Fast
45
40
35
|G*|sin delta, kPa

30
25
Manufacturer 1
20
15 Manufacturer 2
10 Manufacturer 3
5
0
0 10 20 30
Time (from beginning of cooling), min

8
 DSRs Differ in time=0 Determination
 Test at different thermal history
45
Manufacturer 2 tests
40 about 6 minutes sooner
35
|G*|sin delta, kPa

30
25
Current T315

20 Manufacturer 1
15
Manufacturer 2
10
5 Manufacturer 3
0
0 10 20 30
Time After Reaching Temperature within 0.1 °C, min

9
 Cannon Standard – No Hardening
13 °C 25 °C
100 50
|G*|sin delta, kPa

|G*|sin delta, kPa

80 40
60 30

8 mm
Manufacturer 1 Manufacturer 1
8 mm

40 Manufacturer 2 20 Manufacturer 2
20 Manufacturer 3 10 Manufacturer 3
10 min 10 min
0 0
0 10 20 30 0 10 20 30
Time After Reaching Temperature Time After Reaching Temperature
within 0.1°C, min within 0.1°C, min
100 50
|G*|sin delta, kPa

|G*|sin delta, kPa

80 40
60 30

25 mm
Manufacturer 1 Manufacturer 1
25 mm

40 Manufacturer 2 20 Manufacturer 2
20 Manufacturer 3 10 Manufacturer 3
10 min 10 min
0 0
0 10 20 30 0 10 20 30
Time After Reaching Temperature Time After Reaching Temperature
within 0.1°C, min within 0.1°C, min

13 °C 25 °C 10
 NC-B Asphalt, Little Hardening
13 °C 19 °C
8000 4000
7000 3500
|G*|sin delta, kPa

|G*|sin delta, kPa

6000 3000
5000 6 kPa/min 2500 2.2 kPa/min

8 mm
4000 Manufacturer 1 2000 Manufacturer 1
8 mm

3000 Manufacturer 2 1500 Manufacturer 2

2000 Manufacturer 3 1000 Manufacturer 3
1000 10 min 500 10 min
0 0
0 10 20 30 0 10 20 30
Time After Reaching Temperature Time After Reaching Temperature
within 0.1°C, min within 0.1°C, min
8000 4000
7000 3500
|G*|sin delta, kPa

|G*|sin delta, kPa

6000 3000
5000 2500 0.9 kPa/min

25 mm
4000
2.5 kPa/min 2000
25 mm

Manufacturer 1 Manufacturer 1
3000 Manufacturer 2 1500 Manufacturer 2
2000 Manufacturer 3 1000 Manufacturer 3
1000 10 min 500 10 min
0 0
0 10 20 30 0 10 20 30
Time After Reaching Temperature Time After Reaching Temperature
within 0.1°C, min within 0.1°C, min
13 °C 19 °C 11
 NC-D Asphalt, Some Hardening
19 °C 25°C
8000 5000
7000
|G*|sin delta, kPa

|G*|sin delta, kPa

6000 4000
5000 13 kPa/min 3000 5.2 kPa/min

8 mm
4000 Manufacturer 1 Manufacturer 1
8 mm

3000 Manufacturer 2 2000 Manufacturer 2

2000 Manufacturer 3 1000 Manufacturer 3
1000 10 min 10 min
0 0
0 10 20 30 0 10 20 30
Time After Reaching Temperature Time After Reaching Temperature
within 0.1°C, min within 0.1°C, min
8000 5000
7000
|G*|sin delta, kPa

|G*|sin delta, kPa

6000 4000
5000 9.4 kPa/min 3000 3.6 kPa/min

25 mm
4000 Manufacturer 1 Manufacturer 1
25 mm

3000 Manufacturer 2 2000 Manufacturer 2

2000 Manufacturer 3 1000 Manufacturer 3
1000 10 min 10 min
0 0
0 10 20 30 0 10 20 30
Time After Reaching Temperature Time After Reaching Temperature
within 0.1°C, min within 0.1°C, min
19 °C 25 °C 12
 Early Observation

1. Older instruments challenged with experiment

2. Instruments differ in approach to conditioning time
3. Conditioning time for 25mm plates shorter than for 8mm
4. Hardening/conditioning time is not a major factor in variability
5. Cannon standard data are much less variable than asphalt data

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 Current Status & Next Steps
• 10 out of 17 labs provided results for stage 1
• TF agreed that sufficient data provided for
phase 1, ready for stage 2  use 10 min

Next Steps
1. Communicate labs with conditioning times
for stage 2
2. Execute stage 2 testing
3. Analyze data and propose updates to T315
4. Report at next ETG
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