LTRC Capsule11-2B Evaluation of Dynamic Shear Rheometer Tests for Emulsions

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PROBLEM Currently, the Louisiana Department of Transportation and Developme nt (LADOTD) requires ductility tests at 25°C according to AASHTO T51 for emulsions and two other tests, namely force ductility ratio at 4°C and elastic recovery at 10°C according to AASHTO T300 and AASHTO T301, respectively, for polymer modified emulsions. The fact that polymer modified asphalt is strain dependent creates questions regarding purchase specifications based on constant strain controlled  tests. In developi ng performance grade (PG) specifications for emulsions, one of the  tests proposed in several reports is th e multiple stress creep recovery (MSCR) test according to ASTM D7405. This test determines percent elastic recovery and non- recoverable creep compliance and measures the damage behavior in the linear and nonlinear range. Compared with the current binder protocol, a repeated creep tests protocol (or some other method that varies the frequency and strain and measures  the accumulated permanent strain of the binder) represents an improvement in the  theoretical and practical concepts that will better rate the binder properties related  to performance. The main objective of this research is to investigate performance related specificatio ns for emulsions through t he use of a Dynamic Shear Rheometer (DSR). The emulsions from selected sources listed in the Qualified Product List of LADOTD will be tested and compared with force ductility and elastic recovery test results. Finally, recommendations will be developed for DSR-based test specifications for emulsion residue. The LADOTD database and literature on different recovery methods will be reviewed and one of the recovery methods will be selected. In addition, the viscosity of the emulsion state will be determined by dynamic viscosity using sinusoidal loading and by steady state viscosity using rotational loading. Multiple protocols will be examined for emulsion and recovered emulsion testing; tests at high, intermediate, and low temperatures will be conducted. One protocol to be tested is the MSCR test using the DSR at a specified temp erature, as recently defined for use in testing for rutting of asphalt binders used in asphalt mixtures. The sample is loaded at constant stress for 1 sec. then allowed to recover for 9 sec. Ten creep and recovery cycles are run at 0.1 kPa creep shear stress followed by 10 at 3.2 kPa creep shear stress. Percent elastic recovery at 0.1 kPa and 3.2 kPa, non-recoverable creep compliance at 0.1 kPa and 3.2 kPa, difference in percent elastic recove ry for the  two creep stresses, and difference in non-recoverable creep complia nce for the two creep stresses will be calculated. The standard protocol will be varied to include Evaluation of Dynamic Shear Rheom eter Tests for Emulsions JUST THE FACTS L T R C  TECHNOLOGY TRANSFER PROGRAM OCTOBER 2010 R E S E A R C H PROJECT CAPSULE 11-2B SPECIAL POINTS OF INTEREST: Problem Addressed Objectives of Research Methodology Used Implementation Potential PROBLEM Start Date: September 1, 2010 Duration:  22 months End Date: June 30, 2012 Funding: SPR: TT-Fed/TT-Re g Principal Investigators:  Nazimuddin Wasiuddin Department of Civil Engineering, Louisiana Tech University William “Bill” King, Jr., P.E. LTRC Asphalt Materials Research Engineer Administrative Contact: Mark J. Morvant, P.E. Associate Director, Research 225-767-9124 Technical Contact: Chris Abadie, P.E. Materials Research Administrator 225-767-9109 OBJECTIVES METHODOLOGY  

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P R O B L E M

Currently, the Louisiana Department of Transportation and Development (LADOTD)

requires ductility tests at 25°C according to AASHTO T51 for emulsions and two

other tests, namely force ductility ratio at 4°C and elastic recovery at 10°C

according to AASHTO T300 and AASHTO T301, respectively, for polymer modified

emulsions. The fact that polymer modified asphalt is strain dependent creates

questions regarding purchase specifications based on constant strain controlled

 tests. In developing performance grade (PG) specifications for emulsions, one of the

 tests proposed in several reports is the multiple stress creep recovery (MSCR) testaccording to ASTM D7405. This test determines percent elastic recovery and non-

recoverable creep compliance and measures the damage behavior in the linear and

nonlinear range. Compared with the current binder protocol, a repeated creep tests

protocol (or some other method that varies the frequency and strain and measures

 the accumulated permanent strain of the binder) represents an improvement in the

 theoretical and practical concepts that will better rate the binder properties related

 to performance.

The main objective of this research is to investigate performance related

specifications for emulsions through the use of a Dynamic Shear Rheometer (DSR).The emulsions from selected sources listed in the Qualified Product List of LADOTD

will be tested and compared with force ductility and elastic recovery test results.

Finally, recommendations will be developed for DSR-based test specifications for

emulsion residue.

The LADOTD database and literature on different recovery methods will be reviewed

and one of the recovery methods will be selected. In addition, the viscosity of the

emulsion state will be determined by dynamic viscosity using sinusoidal loading and

by steady state viscosity using rotational loading. Multiple protocols will be

examined for emulsion and recovered emulsion testing; tests at high, intermediate,and low temperatures will be conducted. One protocol to be tested is the MSCR test

using the DSR at a specified temperature, as recently defined for use in testing for

rutting of asphalt binders used in asphalt mixtures. The sample is loaded at

constant stress for 1 sec. then allowed to recover for 9 sec. Ten creep and recovery

cycles are run at 0.1 kPa creep shear stress followed by 10 at 3.2 kPa creep shear

stress. Percent elastic recovery at 0.1 kPa and 3.2 kPa, non-recoverable creep

compliance at 0.1 kPa and 3.2 kPa, difference in percent elastic recovery for the

 two creep stresses, and difference in non-recoverable creep compliance for the two

creep stresses will be calculated. The standard protocol will be varied to include

Evaluation of Dynamic Shear Rheometer Testsfor Emulsions

J U S T T H E F A C T S

LTRC 

T E C H N O L O G Y T R A N S F E R P R O G R A M

O C T O B E R 2 0 1 0

R E S E A R C H

P R O J E C T C A P S U L E 11-2B

S P E C I A L P O I N T S O F

I N T E R E S T :

Problem Addressed

Objectives of Research

Methodology Used

Implementation Potential

P R O B L E MStart Date: 

September 1, 2010

Duration: 

22 months

End Date: 

June 30, 2012

Funding:SPR: TT-Fed/TT-Reg

Principal Investigators: 

Nazimuddin Wasiuddin

Department of Civil Engineering,

Louisiana Tech University

William “Bill” King, Jr., P.E.

LTRC Asphalt Materials Research

Engineer

Administrative Contact: 

Mark J. Morvant, P.E.

Associate Director, Research

225-767-9124

Technical Contact: 

Chris Abadie, P.E.

Materials Research Administrator

225-767-9109

O B J E C T I V E S

M E T H O D O L O G Y  

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stress limits such as 50 Pa, 100 Pa, 300 Pa, 500 Pa, 1000 Pa, 3000 Pa, 5000 Pa, and 10,000 Pa and

 temperatures of 10°C, 25°C, and high pavement temperatures to evaluate commonly used LADOTD emulsions.

The scope of this research includes: MSCR testing for polymer identification, strain sweep for non-linearity,

frequency sweep for aged brittleness, and G*/sinδ for stiffness/bleeding. A multiple strain fatigue test will also be

examined. The behavior of emulsion residue will be represented with a viscoelastic material model to fit data

generated in this study.

In 2008, Gayle King proposed a “Strawman” PG specification for emulsions that included MSCR, eliminating float,

penetration, ductility, elastic recovery, and other tests. The proposed specification was revised in 2009; however,

none of the older tests were included in the revised version. Simply eliminating elastic recovery and force ductility

will save enough time to justify the cost of a rheometer needed for the proposed purchase specification tests.

Moreover, rheological test based specifications drive towards improved methods that are more mechanistic and

 that simulate real conditions. To this end, this proposal has been prepared to study the applicability of the MSCR

 test along with a set of DSR-based test methods including a viscosity test, frequency sweep test, and strain sweep test to replace force ductility and an elastic recovery test for emulsions.

Page 2R E S E A R C H

P R O J E C T C A P S U L E 11-2B

Lou is iana Transpor ta t ion Research Center   sponsored jointly by the

Lou i si ana Depa r tm en t o f T ranspo r ta t i on & Deve lopm en t & Lou i si ana Sta te Un i ve rs i t y   

4101 Gourrier Avenue Baton Rouge, LA 70808-4443

For more information about LTRC’s research program, please visit our Web site. w w w . l t r c . l s u . e d u   

I M P L E M E N T A T I O N P O T E N T I A L

DSR: AR2000ex Rheometer