Technical Report Documentation Page

1. Report No. 2. Government Accession No. 3. Recipient’s Catalog No.

FHWA DTFH-61-06-H-00011
4. Title and Subtitle 5. Report Date
Developing a Simple and Rapid Test for Monitoring the Heat Evolution of Concrete April 2008
Mixtures for Both Laboratory and Field Applications-Phase III 6. Performing Organization Code

7. Author(s) 8. Performing Organization Report No.

Kejin Wang, J. Mauricio Ruiz, Jiong Hu, Zhi Ge, Qinwu Xu, Jim Grove, and Rob
Rasmussen
9. Performing Organization Name and Address 10. Work Unit No. (TRAIS)
National Concrete Pavement Technology Center
Iowa State University 11. Contract or Grant No.
2711 South Loop Drive, Suite 4700
Ames, IA 50010-8664
12. Sponsoring Organization Name and Address 13. Type of Report and Period Covered
Federal Highway Administration Final Report
U.S. Department of Transportation 14. Sponsoring Agency Code
400 7th Street SW
Washington, DC 20590
15. Supplementary Notes
Visit www.cptechcenter.org for color PDF files of this and other research reports.
16. Abstract
The objective of this research project is to identify, develop, and evaluate a simple, economical, and reliable calorimetry device and test
method for monitoring heat evolution of pavement concrete. The project contains three phases: phase I—identifying user needs for
calorimeter tests, phase II—identifying potential calorimeter devices and developing test procedures, and phase III—verifying the test
procedures and the potential applications of calorimetry in field. In this report, the work done in phases I and II is briefly summarized
and the study of phase III is presented.

The phase III study includes three parts: (1) field calorimetry tests, (2) lab tests for the field materials, and (3) implementation of
calorimetry into pavement performance prediction. The field tests were conducted at three selected sites: US 71 (Atlantic, Iowa),
Highway 95 (Alma Center, Wisconsin), and US 63 bypass (Ottumwa, Iowa). A simple isothermal calorimetry and two semi-adiabatic
calorimetry (AdiaCal and IQ drum) tests were conducted at these sites. The general concrete, such as slump, air content, unit weight,
placement temperature, ASTM C403 set time, and pavement properties, such as subbase temperature and sawing time were also
measured. In the lab tests of the field materials, nine robust mixes for each field site, with different variations in water reducer and/or fly
ash dosages were developed. AdiaCal and isothermal calorimeter tests were performed for each of the robust mixes. IQ drum and
ASTM C403 set time tests were conducted for selected mixes. To implement the calorimetry test results into concrete performance
prediction, the HIgh PERformance PAVing (HIPERPAV) computer program was modified, the calculated hydration curve parameters
from selected calorimetry tests were used as inputs for the modified HIPERPAV program, and the temperature developments of in-situ
pavements were then predicted. The phase III test results confirmed the major findings drawn in the phase II study. The results indicate
that both the AdiaCal and semi-adiabactic calorimetry tests can provide valuable information on concrete performance. AdiaCal
calorimetry is particularly good for field concrete set time prediction, and it is sensitive to the sample temperature. Isothermal
calorimetry can provide users more detailed information on cement hydration and provide more consistent test results. The thermal set
times obtained from both the AdiaCal and isothermal calorimetry tests are closely related to those measured from the ASTM C403 tests.
Using the calorimetry test curve as inputs for the HIPERPAV computer program, in-situ concrete pavement temperatures can be
predicted adequately.

17. Key Words 18. Distribution Statement

calorimeter— concrete maturity—heat evolution —heat evolution curves—HIPERPAV No restrictions.
isothermal testing—semi-adiabatic testing—software

19. Security Classification (of this report) 20. Security Classification (of this page) 21. No. of Pages 22. Price
Unclassified. Unclassified. 188 NA

v
vi
 DEVELOPING A SIMPLE AND RAPID TEST FOR
MONITORING THE HEAT EVOLUTION OF CONCRETE
MIXTURES FOR BOTH LABORATORY AND FIELD
APPLICATIONS-PHASE III
Final Report
April 2008

Principal Investigator
Kejin Wang, Associate Professor
Department of Civil, Construction and Environmental Engineering
Iowa State University

Co-Principal Investigators
Jim Grove
National Concrete Pavement Technology Center
Iowa State University

J. Mauricio Ruiz
Transtec Group

Rob Rasmussen
Transtec Group

Research Assistant
Zhi Ge
Jiong Hu
Qinwu Xu

Authors
Kejin Wang, J. Mauricio Ruiz, Jiong Hu, Zhi Ge, Qinwu Xu, Jim Grove, and Rob Rasmussen

Sponsored by
the Federal Highway Administration
DTFH-61-06-H-00011
(W04)

A report from
National Concrete Pavement Technology Center
Center for Transportation Research and Education
Iowa State University
2711 South Loop Drive, Suite 4700
Ames, IA 50010-8664
Phone: 515-294-8103
Fax: 515-294-0467
www.cptechcenter.org

vii
v
 TABLE OF CONTENTS

TABLE OF CONTENTS................................................................................................................V

LIST OF FIGURES ..................................................................................................................... VII

LIST OF TABLES..........................................................................................................................X

ACKNOWLEDGMENTS ..........................................................................................................XIII

EXECUTIVE SUMMARY ....................................................................................................... XIV

1. INTRODUCTION .......................................................................................................................1
1.1 Research Background ....................................................................................................1
1.2 Research Approach and Scope.......................................................................................1
1.3 Summary of Phase I and II Study ..................................................................................2
1.4 Description of Phase III Study.......................................................................................3

2. FIELD SITE SELECTION AND DESCRIPTION .....................................................................5

2.1 Field Site Selection ........................................................................................................5
2.2 Mix Proportions .............................................................................................................7
2.3 Material Properties.........................................................................................................8

3. FIELD TESTS AND RESULTS ...............................................................................................10

3.1 Tests and Methods .......................................................................................................10
3.2 Test Results..................................................................................................................12
3.3 Comparison of Field Test Results from Different Projects .........................................39

4. LAB TESTS FOR FIELD CONCRETE MATERIALS............................................................43

4.1 Tests and Methods .......................................................................................................43
4.2 Results and Discussion ................................................................................................46
4.3 Comparison of Lab Test Results from Different Projects ...........................................74

5. HIPERPAV PREDICTION OF CONCRETE PERFORMANCE ............................................78

5.1 Introduction..................................................................................................................78
5.2 Activation Energy ........................................................................................................79
5.3 Hydration Curve Parameters Based on Isothermal Test ..............................................83
5.4 Hydration curve parameters based on the semi-adiabatic test and HIPERPAV II
model..................................................................................................................................94
5.5 Conversion from Isothermal to Semi-Adiabatic Calorimetry......................................99
5.6 Modification of HIPERPAV Software ......................................................................109

v
 5.7 Prediction of Pavement Temperatures .......................................................................111
5.8 Conclusion .................................................................................................................122

6. SPECIFICATION MODIFICATION......................................................................................124

7. CONCLUSIONS AND RECOMMENDATIONS ..................................................................125

8. REFERENCES ........................................................................................................................128

APPENDIX A: INFORMATION OF FIELD PROJECTS ........................................................ A-1

A.1 Information for Atlantic Project............................................................................... A-1
A.2 Information for Alma Center Project ....................................................................... A-7
A.3 Information for Ottumwa Project........................................................................... A-14

APPENDIX B. ADIACAL MORTAR ROBUST TEST RESULTS SUMMARY.....................B-1

APPENDIX C. ISOTHERMAL MORTAR ROBUST TEST RESULTS SUMMARY.............C-1

APPENDIX D: CALIBRATION OF THE CALORIMETER ................................................... D-1

APPENDIX E: PROPOSED SPECIFICATION FOR MONITORING HEAT EVOLUTION OF

CEMENTITIOUS MATERIALS USING A SIMPLE ISOTHERMAL CALORIMETRY
TECHQUE (VERSION 2)...............................................................................................E-1
E.1 Scope .........................................................................................................................E-1
E.2 Referenced Documents..............................................................................................E-1
E.3 Summary of Test Method..........................................................................................E-2
E.4 Significance and Use .................................................................................................E-2
E.5 Apparatus...................................................................................................................E-2
E.6 Test Specimens..........................................................................................................E-3
E.7 Procedure...................................................................................................................E-3
E.8. Calculations ..............................................................................................................E-4
E.9 Report ........................................................................................................................E-6
E.10 Precision and Bias ...................................................................................................E-6

vi
 LIST OF FIGURES

Figure 1. Location of the Atlantic project........................................................................................5

Figure 2. Location of the Alma Center project ................................................................................6
Figure 3. Location of the Ottumwa project......................................................................................6
Figure 4. Water to cement ratio for the mixes of US 71 (Atlantic project) ...................................13
Figure 5. AdiaCal calorimeter........................................................................................................15
Figure 6. AdiaCal test results and determination of the set times .................................................16
Figure 7. ASTM set time vs. AdiaCal thermal set time from US 71 (Atlantic, IA) field study
(Initial thermal set—17% and 14% fraction for two AdiaCal, respectively; Final thermal
set—50% fraction for both AdiaCal).................................................................................17
Figure 8. Isothermal calorimetry results for US 71 (Atlantic, IA) field mortar samples...............18
Figure 9. Isothermal calorimetry results for US 71 (Atlantic, IA) field concrete samples............18
Figure 10. Heat evolution with time for US 71 (Atlantic, IA) field test........................................19
Figure 11. Maturity-strength relationship for US 71 (Atlantic, IA) samples.................................20
Figure 12. Pavement temperature from US 71 (Atlantic, IA) field tests .......................................21
Figure 13. Pavement temperature from US 71 (Atlantic, IA) measured at the middle on different
date.....................................................................................................................................22
Figure 14. Water to cement ratio for the mixes of HW 95 (Alma Center, WI) project.................22
Figure 15. ASTM set time vs. AdiaCal thermal set for HW 95 (Alma Center, WI) project, 18%
fraction for initial thermal set and 41% for final thermal set.............................................26
Figure 16. Temperature from AdiaCal tests (tests were performed on HW 95, July 18th)............27
Figure 17. Isothermal calorimetry results from HW 95 (Alma Center, WI) field study ...............28
Figure 18. Heat evolution with time for HW 95 (Alma Center, WI) project field test..................29
Figure 19. Maturity-strength relationship for HW 95 (Alma Center, WI) samples ......................30
Figure 20. Pavement temperature for HW 95 (Alma Center, WI) project ....................................31
Figure 21. Water to cement ratio for the mixes of US 63 bypass (Ottumwa, IA) project .............32
Figure 22. ASTM set time vs. AdiaCal thermal set for US 63 bypass (Ottumwa, IA) project—
13% fraction for initial thermal set and 49% for final thermal set ....................................34
Figure 23. Isothermal calorimetry results for US 63 bypass (Ottumwa, IA) project.....................36
Figure 24. Heat evolution with time for US 63 bypass (Alma Center, WI) project ......................37
Figure 25. Pavement temperature for US 63 bypass (Ottumwa, IA) project.................................38
Figure 26. ASTM set time vs. AdiaCal thermal set time—initial set ............................................39
Figure 27. ASTM set time vs. AdiaCal thermal set time—final set ..............................................40
Figure 28. Summary of isothermal field calorimetry results .........................................................41
Figure 29. Pavement sawing time vs. AdiaCal thermal final set time...........................................42
Figure 30. AdiaCal robust test results of US 71 (Atlantic, IA) concrete mixes ............................47
Figure 31. Estimated set time from US 71 (Atlantic, IA) AdiaCal robust test ..............................47
Figure 32. Areas under AdiaCal test curves of US 71 (Atlantic, IA) project during different test
period .................................................................................................................................48
Figure 33. Statistical analysis from US 71 (Atlantic, IA) AdiaCal robust test..............................49
Figure 34. Isothermal test results of US 71 (Atlantic, IA) Mix 1 at four temperatures.................50
Figure 35. Isothermal robust test results of US 71 (Atlantic, IA) mortar mixes at different
temperatures.......................................................................................................................52
Figure 36. Estimated set time from isothermal robust test on US 71 (Atlantic, IA) mixes...........52
Figure 37. Heat generation from isothermal robust test mixes at different times US 71 (Atlantic,

vii
 IA) mixes ...........................................................................................................................53
Figure 38. Effect of mix design and temperature on IS and FS from isothermal robust test US 71
(Atlantic, IA mixes) ...........................................................................................................54
Figure 39. IQ drum test result of US 71 (Atlantic, IA) Mix 1 .......................................................55
Figure 40. AdiaCal robust test results of HW 95 (Alma Center, WI) mortar mixes .....................55
Figure 41. Estimated set time from HW 95 (Alma Center, WI) AdiaCal robust test....................56
Figure 42. Areas under HW 95 (Alma Center, WI) AdiaCal test curves during different test
period .................................................................................................................................57
Figure 43. Statistical analysis from the HW 95 (Alma Center, WI) AdiaCal robust test..............57
Figure 44. Isothermal test results of HW 95 (Alma Center, WI) mortar mix 1 at different
temperatures.......................................................................................................................58
Figure 45. Isothermal test results of HW 95 (Alma Center, WI) mortar mixes different
temperatures.......................................................................................................................60
Figure 46. Estimated set time from isothermal robust test on HW 95 (Alma Center, WI) mixes.61
Figure 47. Heat generation from isothermal robust test mixes at different times HW95 (Alma
Center, WI) mixes..............................................................................................................61
Figure 48. Effect of mix design and temperature on IS and FS from isothermal robust test HW 95
(Alma Center, WI) mixes...................................................................................................62
Figure 49. Isothermal test results of mortar with normal and overdosed chemical admixtures ....63
Figure 50. IQ Drum test result of the HW 95 (Alma Center, WI) concrete (Mix 1) .....................64
Figure 51. AdiaCal robust test results of US 63 bypass (Ottumwa, IA) concrete mixes...............65
Figure 52. Estimated set time from US 63 bypass (Ottumwa, IA) AdiaCal robust test ................66
Figure 53. Areas under AdiaCal test curves of US 63 bypass (Ottumwa, IA) projects during
different test period ............................................................................................................66
Figure 54. Statistical analysis from the US 63 bypass (Ottumwa, IA) AdiaCal robust test ..........67
Figure 55. Isothermal test results for US 63 bypass (Ottumwa, IA) mix 1 at different
temperatures.......................................................................................................................68
Figure 56. Isothermal robust test results of US 63 (Ottumwa, IA) mortar mixes at different
temperatures.......................................................................................................................69
Figure 57. Estimated set time from isothermal robust test on US 63 bypass (Ottumwa, IA) mixes70
Figure 58. Heat generation from isothermal robust test mixes at different times US 63 bypass
(Ottumwa, IA) mixes .........................................................................................................71
Figure 59. Effect of mix design and temperature on IS and FS from isothermal robust test (US63
bypass (Ottumwa, IA) mixes) ............................................................................................72
Figure 60. IQ Drum test result of US 63 bypass (Ottumwa, IA) Mix 1 ........................................73
Figure 61. Effect of mix design on ASTM setting time US63 bypass (Ottumwa, IA) mixes .......74
Figure 62. AdiaCal calorimetry results from different projects (Mix 1) .......................................75
Figure 63. Isothermal test results of mortar mix 1 of three projects at different temperatures .....76
Figure 64. Comparison of isothermal and AdiaCal set time results ..............................................77
Figure 65. Comparison of ASTM and thermal set time results .....................................................77
Figure 66. Locate maximum hydration rate...................................................................................79
Figure 67. Determine a linear relationship ....................................................................................80
Figure 68. Activation energy calculation for AlmaCenter site (nine mixes, at four temperatures: 5
o
C, 20 oC, 30 oC, and 40oC; P unit: mW/g; T unit: K)........................................................81
Figure 69. Activation energy calculation for Atlantic site (nine mixes, at four temperatures: 10
o
C, 20 oC, 30 oC, and 40oC; P unit: mW/g; T unit: K)........................................................82

viii
Figure 70. Activation energy calculation for Ottumwa site (nine mixes, at four temperatures: 10
o
C, 20 oC, 30 oC, and 40oC; P unit: mW/g; T unit: K)........................................................82
Figure 71. Calculated activation energies for nine mixes at three sites based on the isothermal
test results...........................................................................................................................83
Figure 72. Influence of hydration curve parameter αu on degree of hydration .............................85
Figure 73. Influence of hydration curve parameter β on degree of hydration ...............................85
Figure 74. Influence of hydration curve parameter τ on degree of hydration................................86
Figure 75. Pre-process the data of rate of heat evolution from isothermal tests............................87
Figure 76. Heat computation based on the trapezoidal method.....................................................88
Figure 77. Predicted degree of hydration vs. measurements at 5 oC (Sample 5, Alma Center) ....89
Figure 78. Theoretical degree of hydration vs. measurements at 20 oC (Sample 5, Alma Center)89
Figure 79. Predicted degree of hydration vs. measurements at 30 oC (Sample 5, Alma Center) ..90
Figure 80. Predicted degree of hydration vs. measurements at 40 oC for (Sample 5, Alma Center)90
Figure 81. Alma Center field concrete...........................................................................................96
Figure 82. Alma Center lab concrete .............................................................................................97
Figure 83. Atlantic Field concrete .................................................................................................98
Figure 84. Ottumwa Field Concrete...............................................................................................99
Figure 85. P vs. Q ........................................................................................................................101
Figure 86. Exponential equations to approximate P vs. Q...........................................................102
Figure 87. Extract P points at any Q state....................................................................................103
Figure 88. Approximate P vs. T at any heat (Q) state..................................................................103
Figure 89. Heat conduction in the calorimeter wall.....................................................................104
Figure 90. Calculated temperature losses versus measurement estimations................................106
Figure 91. Heat generation of cementitious material...................................................................107
Figure 92. Simulated semi-adiabatic temperature (from isothermal data) vs. measurements .....108
Figure 93. Flow chart of computation procedure.........................................................................109
Figure 94. Windows of inputs of hydration curve parameters in the modified HIPERPAV II
software............................................................................................................................110
Figure 95. Temperature at the Alma Center, IA ..........................................................................111
Figure 96. Wind speed at the Alma Center, IA............................................................................112
Figure 97. Humidity at the Alma Center, IA ...............................................................................112
Figure 98. Predicted pavement temperatures versus measurements (pavement top, Alma Center,
WI ) ..................................................................................................................................113
Figure 99. Predicted pavement temperatures versus measurements (pavement mid, Alma Center,
WI) ...................................................................................................................................114
Figure 100. Predicted pavement temperatures versus measurements (pavement bottom, Alma
Center, WI) ......................................................................................................................114
Figure 101. Temperature in Atlantic, IA .....................................................................................115
Figure 102. Wind Speed in Atlantic, IA ......................................................................................116
Figure 103. Humidity in Atlantic, IA...........................................................................................116
Figure 104. Predicted pavement temperatures versus measurements (pavement top, Atlantic, IA)117
Figure 105. Predicted pavement temperatures versus measurements (pavement mid, Atlantic, IA)118
Figure 106. Predicted pavement temperatures versus measurements (pavement mid, Atlantic, IA)118
Figure 107. Temperature in Ottumwa, IA ...................................................................................119
Figure 108. Wind speed in Ottumwa, IA.....................................................................................120
Figure 109. Humidity in Ottumwa, IA.........................................................................................120

ix
Figure 110. Predicted pavement temperatures versus measurements (pavement top, Ottumwa,
IA) ....................................................................................................................................121
Figure 111. Predicted pavement temperatures versus measurements (pavement mid, Ottumwa,
IA) ....................................................................................................................................121
Figure 112. Predicted pavement temperatures versus measurements (pavement bottom, Ottumwa,
IA) ....................................................................................................................................122

LIST OF TABLES

Table 1. Mix design for Atlantic project..........................................................................................7

Table 2. Mix design for Alma Center project ..................................................................................7
Table 3. Mix design for Ottumwa project........................................................................................8
Table 4. Chemical properties of cement ..........................................................................................8
Table 5. Chemical properties of fly ash ...........................................................................................8
Table 6. Aggregate specific gravity and absorption ........................................................................9
Table 7. Concrete and pavement information for US 71 (Atlantic project) ..................................14
Table 8. Concrete and pavement information for HW 95 (Alma Center, WI) project ..................24
Table 9. Concrete and pavement information for US 63 bypass (Ottumwa, IA) project ..............33
Table 10. Concrete mix proportions for US 71 project (Atlantic, IA)...........................................44
Table 11. Concrete mix proportions for the HW95 project (Alma Center, WI)............................44
Table 12. Concrete mix proportions for US 63 bypass project (Ottumwa. IA).............................45
Table 13. ASTM set time result from robust test (US 63 (Ottumwa, IA) mixes) .........................73
Table 14. Calculated activation energy (Unit: J/mol)....................................................................83
Table 15. Hydration curve parameters calculated based on isothermal test results (Alma Center,
WI) .....................................................................................................................................91
Table 16. Hydration curve parameters back-calculated based on isothermal test results (Atlantic,
IA) ......................................................................................................................................92
Table 17. Hydration curve parameters back-calculated based on isothermal test results
(Ottumwa, IA)....................................................................................................................93
Table 18. Sensitivity of hydration curve parameters to total heat .................................................94
Table 19. Back-calculated hydration curve parameters based on Semi-adiabatic test ..................99
Table B.1. Summary of AdiaCal robust test results of US 71 (Atlantic, IA) mixes....................B-1
Table B.2. Summary of AdiaCal robust test results of HW 95 (Alma Center, WI) mixes..........B-1
Table B.3. Summary of AdiaCal robust test results of US 63 bypass (Ottumwa , IA) mixes.....B-2
Table C.1. Summary of isothermal robust test results of US 71 (Atlantic, IA) mortar mixes at
10oC..................................................................................................................................C-1
Table C.2. Summary of isothermal robust test results of US 71 (Atlantic, IA) mortar mixes at
20oC..................................................................................................................................C-1
Table C.3. Summary of isothermal robust test results of US 71 (Atlantic, IA) mortar mixes at
30oC..................................................................................................................................C-2
Table C.4. Summary of isothermal robust test results of US 71 (Atlantic, IA) mortar mixes at
40oC..................................................................................................................................C-2
Table C.5. Summary of isothermal robust test results of HW 95 (Alma Center, WI) mortar mixes
at 5oC................................................................................................................................C-3
Table C.6. Summary of isothermal robust test results of HW 95 (Alma Center, WI) mortar mixes
at 20oC..............................................................................................................................C-3

x
Table C.7. Summary of isothermal robust test results of HW 95 (Alma Center, WI) mortar mixes
at 30oC..............................................................................................................................C-4
Table C.8. Summary of isothermal robust test results of HW 95 (Alma Center, WI) mortar mixes
at 40oC..............................................................................................................................C-4
Table C.9. Summary of isothermal robust test results of US 63 bypass (Ottumwa, IA) mortar
mixes at 10oC ...................................................................................................................C-5
Table C.10. Summary of isothermal robust test results of US 63 bypass (Ottumwa, IA) mortar
mixes at 20oC ...................................................................................................................C-5
Table C.11. Summary of isothermal robust test results of US 63 bypass (Ottumwa, IA) mortar
mixes at 30oC ...................................................................................................................C-6
Table C.12. Summary of isothermal robust test results of US 63 bypass (Ottumwa, IA) mortar
mixes at 40oC ...................................................................................................................C-6
Table C.13. Summary of robust isothermal test results of US 71 (Atlantic, IA) mixes ..............C-7
Table C.14. Summary of robust isothermal test results of HW 95 (Alma Center, WI) mixes ....C-7
Table C.15. Summary of robust isothermal test results of US 63 bypass (Ottumwa, IA) mixes C-8

xi
xii
ACKNOWLEDGMENTS

This project is sponsored by the National Concrete Pavement Technology Center (CP Tech
Center) and the Federal Highway Administration (FHWA). The authors would like to express
their gratitude to the CP Tech Center and FHWA for their support.

Special thanks are extended to the technical working group (TWG) members:
• Paul Sandberg (W.R. Grace)
• Wes Woytowich (Lafarge)
• Anton Schindler (Auburn University)
• Todd Hanson (Iowa Department of Transportation)
• Tim Cost, Gary Knight, and Steve Otto (Holcim)
• Gary Crawford (Federal Highway Administration)
• Leif Wathne (American Concrete Pavement Association)
• Karthia Obla (National Ready Mixed Concrete Association)
• Heather Houck (National Ready Mixed Concrete Association)
• Geoffrey Kurgan (Federal Highway Administration)

The authors are particularly indebted to Sandberg for his valuable advice on the use of
calorimeter equipment and test data analyses and to Lafarge, Holcim, and CTL Group for
providing the project with cementitious materials.

Finally, the authors would like to thank Bob Steffes, Gang Lu, and Gilson Lomboy at Iowa State
University for their great help in the lab. The project might not have been completed on schedule
without the support from all the individuals listed above.

xiii
xiv
EXECUTIVE SUMMARY

Concrete quality control is critical for ensuring desired field concrete performance. A number of
quality control test methods have been developed and some of them are routinely used in field.
The test methods include slump, air content, and strength/maturity tests. Lately, various tests
(such as false set, rheological, and calorimetry tests) are also developed for identifying the
incompatibility of supplementary cementitious materials and chemical admixtures in concrete.
Among these existing test methods, some of them are too simple to be accurate and some of
them require expensive equipment, complex testing procedures, and/or extensive time, thus are
not suitable for field application. Since cement hydration process directly influences concrete
workability, setting behavior, strength gain rates, and microstructure development, it is believed
that the deviations in the quantities and characteristics of the concrete constituents as well as
effects of construction conditions can be detected and concrete performance can be predicted by
one test—a calorimetry test—that monitors the heat of cement hydration in concrete.

The objective of the present research is to identify, develop, and evaluate a simple, economical,
and reliable calorimetry device and test method for monitoring heat evolution of pavement
concrete. This research project contains three phases:
Phase I: Identifying user needs for calorimeter tests, potential applications of calorimeter test
results, and a potential calorimeter device for the phase II study (completed in December 2005)
Phase II: Developing test procedures and methods for interpreting the test results (completed in
December 2007)
Phase III: Verifying the test procedures and the potential applications of calorimetry in field

In this report, the work done in phases I and II is briefly summarized and the study of phase III is
presented. The phase III study includes three major parts: (1) field tests, (2) lab tests for the field
materials, and (3) implementation of calorimetry into HIgh PERformance concrete PAVing
(HIPERPAV) prediction. Three field sites, US 71 (Atlantic, Iowa), Highway 95 (Alma Center,
Wisconsin), and US 63 bypass (Ottumwa, Iowa) were selected, and calorimetry tests were
conducted at these field sites using different calorimeters: a simple isothermal calorimeter, as
identified in the phase II study, and two semi-adiabatic calorimeters (AdiaCal and IQ drum). The
set times of the field concrete were also measured according to ASTM C403, and general
properties of the concrete and pavement (such as concrete slump, air content, unit weight,
water/cement ratio [w/c], placement temperature, and pavement subbase temperature and sawing
time) were also recorded. Robust tests were conducted in lab for these field concrete materials.
Nine robust mixes for each field project, with 50% variations in water reducer (WR) and/or fly
ash (FA) dosages from the mix proportion actually used in field were developed and studied.
AdiaCal tests were performed for each robust mix, and isothermal calorimeter tests were
performed for each robust mix at four different temperatures. Selected IQ drum tests and ASTM
C403 set time tests were also performed in lab so as to compare the lab results with the field test
results. A statistical analysis was conducted to analyze these test data. The activation energies are
determined from the isothermal test results of heat signatures using the Arrhenius equation.
Hydration curve parameters are back-calculated from both the isothermal tests and semi-
adiabatic tests. Then the back-calculated hydration curve parameters are input into the
HIPERPAV computer program which is modified to offer a window for users to define and input
those parameters, in order to predict the pavement performance including the temperature in the

xv
in situ pavements and associated strength and stress development. A mathematical model and
associated computation approach are also developed to convert the isothermal signature of
cement mortar to the semi-adiabatic signature of cement concrete.

The results of the field tests conducted in the phase III study indicate the following:
• AdiaCal semi-adiabactic calorimetry tests, using concrete samples, can provide general
information on concrete performance. The test results are very sensitive to the concrete
placement temperature. (The temperature curves obtained from the AdiaCal calorimeter tests
varied largely in the samples tested in the same day.) Thus, the test results are useable for set
time prediction of field concrete but not desirable for accurate concrete quality control.
• Similar to the findings drawn in the phase II study, the thermal set times obtained from both
AdiaCal and isothermal calorimetry tests are closely related to those from the ASTM C403
tests. Compared with the isothermal calorimetry test, the AdiaCal test is easy to operate.
• The simple isothermal calorimetry test results of samples at a given project were consistent.
The test results of samples from different projects looked very different, demonstrating the
subtle changes in these concrete materials and/or mixture proportions. As a result, the simple
isothermal calorimeter could be a good tool for daily concrete quality control.
• In the simple isothermal calorimetry tests, concrete samples showed much larger variations
than mortar samples. Therefore, mortar samples sieved from field concrete are recommended
for field calorimetry tests.
• No incompatibility problem in the concrete studied was identified by the calorimetry tests.
• Neither the isothermal calorimeter nor AdiaCal showed good ability to identify changes in
w/c ratio of the field concrete. Hence, the microwave method can be used as a supplementary
test for such identification.
• Pavement sawing times were close to the final setting time in these three field projects, but
no clear relationship was observed between the setting and sawing times.

The results from the lab tests for the field materials suggest the following:
• The results from the lab tests for the field materials are generally consistent with those from
the corresponding field tests.
• The simple isothermal tests showed clearly a second peak related to the hydration of fly ash
in the concrete mixes tested. Such a heat evolution peak was not generally observed from
AdiaCal or IQ Drum tests.
• The thermal set times obtained form both AdiaCal and isothermal calorimetry tests were
well-related to those from the ASTM C403 tests. The effects of WR dosage and FA
replacement levels on concrete set time could be identified by both calorimetry test methods.
• The simple isothermal tests results illustrated that as testing temperature increased, the
variation in thermal set time decreased. This implies that potential concrete set time and
strength development problems might show in winter construction while fewer problems
may be expected in summer construction.
• Testing/curing temperature had a more significant effect on concrete calorimetry parameters
(thermal set time and the area under the heat evolution curve) than WR and FA. Compared
with FA, WR has less effect on thermal set time. However, in different projects, WR had
different effects on calorimetry parameters.
• The robust tests demonstrated that when the WR and/or FA amounts are 50% higher or lower
than the designed dosage, the concrete heat-generation curves looked similar but shifted only

xvi
 to the left or right, depending on the degree of the material variation. There was no
incompatibility problem within these mixes tested at the designed testing temperature.
• The robust test method can be used for establishing acceptable heat evolution boundaries.
Thus, field engineers can easily evaluate their calorimetry test results and use the calorimetry
as a single tool for field concrete quality control.

The results from the theoretical models and HIPERPAV implementation indicate the following:
• The computed activation energies of the cementitious materials using the Arrhenius equation
based on the isothermal test data are close to the values reported by other researchers.
• It seems that adding WR and FA replacement increases activation energy.
• The hydration curve parameter αu increases, while β and τ decrease when decreasing the total
heat of hydration Hu based on the isothermal test data.
• The calculated hydration curve parameter β, based on the isothermal test data, seems to be
larger than that based on the semi-adiabatic test data, while the hydration curve parameter τ
based on the isothermal test data seems to be smaller than that based on the semi-adiabatic
test data.
• The simulated semi-adiabatic temperatures in terms of the isothermal heat signatures have a
reasonable agreement with the measurements though there is some small delay at the early
stage.
• The hydration curve parameters resulting from semi-adiabatic test data (as opposed to
isothermal test data) are a better match to actual portland cement concrete (PCC) pavement
temperatures. This result could be due to at least two reasons: (1) the semi-adiabatic test
condition is closer to that of the in situ pavements; (2) the semi-adiabatic test is conducted on
concrete as that of in situ pavement, while the isothermal test is conducted on the cement
mortar.

The findings from the present research also imply that proper application of a simple calorimetry
technique in lab and/or field will provide engineers with important information on concrete
quality and performance that may otherwise require conducting many different tests.

xvii
18
1. INTRODUCTION

1.1 Research Background

Concrete quality control is critical for ensuring desired field concrete performance. A number of
quality control test methods have been developed and routinely used in-field over decades, which
include slump, air content, and strength tests. Set time of concrete is sometimes tested in lab to
assist in the determination of the pavement finishing and sawing time. Maturity test methods
have commonly been used in the field as a replacement for concrete strength tests. Due to
increasing applications of various supplementary cementitious materials (SCMs) and admixtures
in modern concrete, various tests (such as false set, rheological and calorimetry tests) are also
developed for identifying the incompatibility of concrete materials. Among these existing test
methods, some of them are too simple to be accurate and some of them require expensive
equipment, complex testing procedures, and/or extensive time, thus are not suitable for field
application. The abnormal cement hydration resulting from “incompatibility” of concrete
materials has resulted in erratic set and strength gain behavior and associated finishing, curing,
and early-age cracking. Influences of construction and environmental conditions, such as cold
and hot weather, often aggravate these problems. However, the existing guidance is lacking on
proper test methods for identifying these problems.

Cement hydration liberates heat. Research has shown that the heat evolution process is strongly
influenced by the chemical and physical properties of portland cement (PC), SCMs, chemical
admixtures, concrete mix proportions, construction procedures, and curing conditions of
concrete. As a result, deviations in the quantities and characteristics of the concrete constituents
as well as effects of construction conditions can be detected and concrete performance can be
predicted by monitoring the heat of cement hydration (1, 2). Recently, the advancements in the
use of thermal measurements of the early heat development of concrete mixtures in the labo-
ratory have demonstrated that calorimetry tests have a high potential for detecting concrete
incompatibility problems, predicting fresh concrete properties (such as setting time), and
assessing hardened concrete performance (such as strength gain and thermal cracking) under
various climatic conditions (3,4).

The objective of this research project is to identify, develop, and evaluate a simple, economical,
and reliable calorimetry device and a test method for monitoring heat evolution of pavement
concrete.

1.2 Research Approach and Scope

This research project consists of three phases:

Phase I: Identifying user needs for calorimeter tests, potential applications of calorimeter test
results, and a potential calorimeter device for the phase II study (completed in
December 2005)
Phase II: Developing test procedures and methods for interpreting the test results (completed in
December 2007)
Phase III: Verifying the test procedures and the potential applications of calorimetry in the field

1
1.3 Summary of Phase I and II Study

In the phase I study, a literature search and a survey of participating agencies and others in the
portland cement concrete (PCC) paving community were conducted to gather information on the
users’ needs for a simple, rapid calorimeter test and the potential applications of calorimeter test
results. The phase I study also included investigations on the existing test procedures for
measuring the heat of hydration of concrete using calorimetry and other methods as well as the
test device. It is concluded that in conjunction with another technology, such as HIgh
PERformance concrete PAVing (HIPERPAV), the heat evolution test results can be used for the
following:
• Flagging changes in cementitious materials
• Prescreening materials and/or mix design
• Identifying incompatibility of cementitious materials
• Verifying mix proportions
• Forecasting setting time
• Estimating sawing and finishing time
• Assessing concrete maturity and strength
• Predicting risk of thermal cracking

After confirming the specific needs of the pavement industry on the calorimetry tests and having
a clear vision on the practical applications of the calorimeter tests, the research team proposed a
focused, systematical study for phase II.

In phase II, two available calorimeter devices, a semi-isothermal calorimeter manufactured by

Thermometric Inc. (approximately $8,000) and a semi-adiabatic calorimeter device, AdiaCal,
(approximately $3,000) were utilized. These devices were selected because they would likely
have a fair cost and produce results that could differentiate the heat signatures of various
concrete materials in a short time span. A wide range of paste and mortar mixtures (over 150
mixes) were tested to evaluate the effects of the concrete materials (ingredients, sources, and
proportions), equipment, and environmental conditions on the calorimetry test results. Some
known incompatible mixes were specially selected and tested. The interpretation methods of the
test results, using the heat evolution indexes that were developed from the derivatives of and the
areas under the heat evolution curves were explored. The relationship between the thermal set
time derived from the calorimetry test results and the ASTM C403 set time test results of
concrete set time and the relationship between the area under the calorimetry curve and the
concrete strength were investigated. A draft of isothermal test specification was developed.

In addition, two field trial tests at New York and South Dakota ware also conducted using the
AdiaCal calorimeter. The research team members at Transtec Group, Inc. also investigated the
potential for predicting concrete performance using results from the calorimetry tests together
with the HIPERPAV computer program. However, due to the limited time and funding, the
phase II study did not include sufficient field tests and HIPERPAV analyses. The phase III study
was then proposed for completing the overall goal of the heat of evolution project.
The following findings were drawn from the phase II study:

2
• The test method developed for the selected isothermal calorimeter device is easy to apply and
repeatable.
• The calorimeter test can be used to differentiate the heat evolution of mortars made with
different materials and subjected to different curing conditions.
• The calorimeter test can be used to identify material incompatibility and to flag cementitious
changes.
• The heat indexes, related to the first derivative of the calorimeter curve and the area under
the curve, are able to characterize the features of mortar. They can also be used to predict the
mortar set time and early-age strength (up to two days).
• The selected semi-adiabatic calorimeter test device (AdiaCal) is also easy to use, and the test
results provide a very good prediction of the set time of field concrete.
• The AdiaCal calorimeter or similar equipment can be modified to compute temperature
losses and can inexpensively replicate the results of semi-adiabatic testing in the field.
• Used with HIPERPAV, semi-adiabatic testing of concrete in the field is the recommended
procedure for prediction of pavement performance characteristics, including set times,
strength gain, and thermal cracking risk.

1.4 Description of Phase III Study

The focus of this report is on the phase III study, which includes three major parts:

1. Field tests
Three field sites, US 71 (Atlantic, Iowa), Highway 95 (Alma Center, Wisconsin), and US
63 bypass (Ottumwa, Iowa) were selected, and calorimetry tests were conducted at
these field sites using different calorimeters: a simple isothermal calorimeter, as
identified in the phase II study, and two semi-adiabatic calorimeter (AdiaCal and IQ
drum). The set times of the field concrete were also measured according to ASTM
C403, and general properties of the concrete and pavement (such as concrete slump,
air content, unit weight, water/cement ratio [w/c]), placement temperature, and
pavement subbase temperature and sawing time) were also recorded.

2. Lab tests for the field materials

Robust tests were conducted in lab for these field concrete materials. Nine robust mixes,
with 50% decrease/increase of water reducer (WR) and/or fly ash (FA) dosages were
developed based on the mix proportion actually used in field for each field project.
AdiaCal tests were performed for each robust mix, and isothermal calorimeter tests
were performed for each robust mix at four different temperatures. Selected IQ drum
tests and ASTM C403 set time tests were also performed in lab so as to compare the
lab results with the field test results. A statistical analysis was conducted to analyze
these test data.

3. Implementation of calorimetry into HIPERPAV prediction

Currently, the HIPERPAV program uses predicted heat evolution results based on cement
characteristics and concrete mix design. Heat evolution information is a fundamental

3
 input to HIPERPAV for the prediction of the pavement strength and risk of thermal
cracking during the early age. This study is to use the calorimeter test results (or heat
evolution indexes) as input data for the HIPERPAV program analysis, thus improving
reliability of the HIPERPAV analysis. The results from the HIPERPAV analysis can
be used for concrete quality control, optimization of pavement designs, and prediction
of pavement performance, and can help contractors in managing the temperature of
concrete based on the concrete mix designs and specific climate and project
conditions.

The detailed information on the phase III research activities and results are presented in the
following sections.

4
2. FIELD SITE SELECTION AND DESCRIPTION

2.1 Field Site Selection

Three field sites (two in Iowa and one in Wisconsin) were selected for the phase III study. The
location and brief description of each field project are presented in the following sections.

2.1.1 US 71 (Atlantic, Iowa)

Figure 1 shows a PCC overlay project on US HWY 71 between US 83 and US 34 at Atlantic,

Iowa. The overlay was 10.56 miles long and constructed using conventional slipform paving
equipment. The 8-in. thick new concrete overlay was placed on top of the partially milled old
asphalt pavement.

Figure 1. Location of the Atlantic project

2.1.2 HW 95 (Alma Center, Wisconsin)

This project is on south HW 95, from I-94 to Alma Center, Wisconsin. The old pavement was
torn up and the new pavement was placed on the old subbase.

5
 Figure 2. Location of the Alma Center project

2.1.3 US 63 bypass (Ottumwa, Iowa)

This project was a new bypass located at Ottumwa, Wapello County, Iowa, from US 63/ IA 149
south to Steller Avenue. The total length of the new pavement is about 17 miles.

Figure 3. Location of the Ottumwa project

6
2.2 Mix Proportions

2.2.1 US 71 (Atlantic, Iowa)

Table 1 shows the mix design for the Atlantic project. The cement used in the project was Type
IP (F) from Ash Grove with a specific gravity of 2.95. The Class C FA was from Headwaters
Inc. with a specific gravity of 2.64. Three types of aggregates (coarse, intermediate, and fine)
were used in this project. The coarse and intermediate aggregate were from Hallet Lakeview,
Iowa. Both of them have specific gravity of 2.70. The fine aggregate was from Hallet Exira,
Iowa. It has a specific gravity of 2.66. The designed air content is 6%. The designed maximum
w/c is 0.45.

Table 1. Mix design for Atlantic project

Materials SSD weight (lbs/cy) Absolute volume (cy)
Cement 442 0.089
Fly ash 110 0.025
Water 221 0.131
Fine aggregate 1309 0.292
Intermediate aggregate 273 0.060
Coarse aggregate 1560 0.343

2.2.2 HW 95 (Alma Center, Wisconsin)

The mix design of Alma Center is listed in Table 3. The cement used in this project is from
Holcim with low alkali. FA is Type C. The moisture was assumed to be 2.5% for sand and 1%
for coarse aggregate during the whole project.

Table 2. Mix design for Alma Center project

Materials SSD weight (lbs/cy)
Cement 446.0
Fly ash 113.0
Water 252.0
Fine aggregate 1370.0
Coarse aggregate 1825.0
AEA-Daravair 5.5 oz
WR-WRDA 82 18.0 oz

7
2.2.3 US63 Bypass (Ottumwa, Iowa)

The mix design was shown in Table 5. The designed air content was 6% and slump was 2 in. The
cement used in this project was Lafarge Type ISM cement. The FA was Type C FA from ISG
Resources Inc. Chillicothe with a specific gravity of 2.73. The coarse aggregate was from Ollie,
Iowa with a specific gravity of 2.66. The fine aggregate was from Eldon, Iowa with a specific
gravity of 2.67. The fineness modulus for the sand was 2.93.

Table 3. Mix design for Ottumwa project

Materials SSD weight (lbs/cy) Absolute volume (cy)
Cement 443.0 0.085
Fly ash 111.0 0.024
Water 222.0 0.132
Fine aggregate 1291.0 0.287
Coarse aggregate 1846.0 0.412
Air-entraining agent 49.1 ml
Water reducer 654.8 ml

2.3 Material Properties

The chemical properties of cement and FA used in three projects are summarized in Table 4 and
Table 5, respectively:

Table 4. Chemical properties of cement

Sample name Na2O MgO Al2O3 SiO2 P2O5 SO3 K2O CaO TiO2 Fe2O3 SrO Mn2O3 LOI
US 71
(Atlantic, IA) 0.30 3.08 8.20 29.64 0.10 3.30 0.73 49.34 0.51 3.31 0.12 0.07 1.29
HW 95
(Alma Center, WI) 0.07 2.35 4.74 20.78 0.08 2.75 0.78 63.09 0.24 3.15 0.11 0.07 1.78
US 63 bypass
(Ottumwa, IA) 0.16 4.30 5.22 23.72 0.10 2.95 0.56 58.79 0.38 2.77 0.04 0.49 0.51

Table 5. Chemical properties of fly ash

Sample name Na2O MgO Al2O3 SiO2 P2O5 SO3 K2O CaO TiO2 Fe2O3 SrO Mn2O3 LOI
US 71
(Atlantic, IA) 1.72 4.63 20.1 34.9 1.01 2.27 0.42 26.2 1.64 5.78 0.42 0.05 0.38
HW 95
(Alma Center, WI) 1.83 5.29 19.1 36.3 1.03 1.93 0.47 25.6 1.53 5.26 0.44 0.03 0.36
US 63 bypass
(Ottumwa, IA) 3.21 6.81 16.2 31.6 1.02 3.13 0.32 28.8 1.24 6.03 0.51 0.02 0.30

Relativity density (specific gravity) and absorptions of the aggregate used in three projects were
tested, and the results are shown in Table 6.

8
Table 6. Aggregate specific gravity and absorption
Sample name Type Gb Gb,SSD Ga Abs., %
US 71 (Atlantic, IA) Fine aggregate Riversand 2.58 2.62 2.69 1.55
Intermediate aggregate Gravel 2.63 2.67 2.75 1.68
Coarse aggregate Gravel 2.67 2.70 2.76 1.20
HW 95 (Alma Center, Fine aggregate Riversand 2.61 2.65 2.72 1.60
WI) Coarse aggregate Quartzite 2.87 2.87 2.89 0.33
US 63 by pass (Ottumwa, Fine aggregate Riversand 2.59 2.62 2.68 1.32
IA) Coarse aggregate Limestone 2.41 2.50 2.64 3.69

9
3. FIELD TESTS AND RESULTS

3.1 Tests and Methods

For each field site, the following tests and information were conducted and recorded:
• Concrete mixing time, dumping time, truck number, subbase temperature
• Pavement paving, finishing, curing, and sawing time
• Air content, slump, and unit weight
• Setting time
• Microwave w/c ratio
• AdiaCal calorimetry test.
• Isothermal calorimetry test
• IQ drum test
• Maturity-strength test

The Concrete Mobile Lab from the Center of Concrete Pavement Technology (CP Tech Center),
Iowa State University (ISU), was brought to three field sites to assist in the field tests.

Concrete mixing time is the time that is shown on the batch ticket. Just before the concrete was
dumped on the ground, the subbase temperature was measured at two positions: the surface of
subbase using the infrared temperature thermometer and about one in. below the surface using
the temperature probe. During the pavement construction, one person stayed in the field and
recorded the paving, finishing, and curing time for the site where concrete was sampled. The
sawing time was recorded by the saw crew when they cut the marked joint.

Concrete was sampled in front of the paver and sent back to the mobile lab to conduct the rest
tests. The air content was conducted following ASTM C231 “Standard Test Method for Air
Content of Freshly Mixed Concrete by the Pressure Method.” The unit weight test followed
ASTM C138 “Standard Test Method for Density (Unit Weight), Yield, and Air Content
(Gravimetric) of Concrete.” The slump test was based on ASTM C143 “Standard Test Method
for Slump of Hydraulic-Cement Concrete.” A maturity and strength test followed ASTM C1074
“Standard Practice for Estimating Concrete Strength by the Maturity Method.” The 4 in. by 8 in.
cylinders were stored in the curing tank of the mobile lab for the first couple days and then
transferred to the curing room at Iowa State University until the testing time. Only one Ibutton
was put in the middle of the concrete sample to record concrete temperature. The cylinders were
broken at 1, 3, 7, 14, and 28 days according to ASTM C39 “Standard Test Method for
Compressive Strength of Cylindrical Concrete Specimens.”

Setting time was performed following ASTM C403 “Standard Test Method for Time of Setting
of Concrete Mixtures by Penetration Resistance.” The mortar samples were sieved from concrete
first. Two tests were conducted on the same concrete for Alma Center and the Ottumwa project
and only one test were performed for the Atlantic project.

10
The sieved mortar was used for the microwave w/c ratio test. About 1500 g of mortar were
placed in a glass bowl and then put in the microwave oven. After being heated for five minutes,
the sample was taken out and weighed and then put back into the microwave oven for another
two minutes. After that the sample was weighed again. If the weight difference between two tests
is less than 0.1 g, the test will stop. Otherwise, the sample was put back into the microwave oven
and heated for two more minutes until the weight difference was less than 0.1 g. The w/c ratio
was calculated based on the data and concrete properties.

The 4 in. by 8 in. cylinders were used for the AdiaCal calorimetry test. The calorimeter was
programmed and keep closed before the concrete samples were prepared. Immediately after the 4
in. by 8 in. samples were loaded into the calorimeter, the lid was closed and the program started
to record concrete temperature. The temperature was recorded every minute by the sensor, which
is located just below the bottom of the sample holder. When the test was finished, the program
was stopped and the data was retrieved from the data logger. For each concrete sample, at least
two cylinders were tested. The thermal set times were determined from each temperature curve
as described below. The average value was used for the data analysis.

Isothermal calorimetry tests were performed for both sieved mortar and concrete samples at each
field site. The test procedures described in the draft of the specification developed in phase II
(Appendix E) were followed closely. However, in the field, the mortar samples were sieved from
the field concrete instead of mixed. Four sieved mortar and concrete samples were tested for
each batch of concrete collected in front of the paver. The mortar sample was about 100 g and
the concrete sample was around 300 g. The tests were done inside the mobile lab and the testing
temperature was maintained at 30°C at all times. The calorimeter was programmed before the
test. The mortar and concrete were put into the plastic container and weighed to the desired
amount. Immediately after the sample was ready, it was loaded into the sample holder of the
isothermal calorimeter. After that the lid was closed, and the test was started. Then the program
recorded the data for every 30 s. When the test was done, the data was retrieved and calibrated.

The cement heat signature test was conducted using the semi-adiabatic calorimeter (IQ drum, as
shown in Figure 3.1) manufactured by Digital Site Systems, Inc., Pittsburgh, Pennsylvania. The
IQ drum consists of (1) a 6 in. by 12 in. cylinder chamber for concrete specimens or a 2 in. by 4
in. cylinder chamber for mortar specimens in the center, (2) a 6 in. layer of insulation materials
outside the chamber, (3) a thermal sensor, and (4) a data logger mounted on the outside wall.
During the test, the thermal sensor is inserted into the concrete/mortar specimen to record the test
data. The semiadiabatic calorimeter allows a certain amount of heat loss during the test period.
The thermal loss can be calculated from the test data and from the calibration factor, which is
determined from a calibration test.

Before each test, the mixing proportion and physical properties of the raw materials were input
into the software, which provided the desired test results regarding the thermal history and the
heat evolution process of the concrete. The concrete obtained from the field was placed into the 6
in. by 12 in. cylinder in three layers and rodded 25 times for each layer. Then, the sample was
weighed and put into the drum along with an inserted sensor. The IQ drum was sealed promptly
after the sample was added. The test data were recorded every 15 minutes with the aid of a

11
computer program. The entire test took about seven days under room conditions. The same
procedure was applied for the mortar sample. But the test for the mortar sample only took three
days.

Tests 1–6 were conducted three rounds each day for the Atlantic project and four rounds for the
Ottumwa and Alma Center project. The isothermal calorimetery test was conducted once each
day because the test has to run for around 24 hours. The maturity-strength test was performed
once for each project. Weather data was recorded for all three projects. However, the data was
lost for the Ottumwa project due to an equipment issue. The IQ drum test was performed once
for each project site on both concrete and mortar samples. The batch ticket for each tested mix
was also collected. For the Atlantic project, it was not able to track the exact mixing time for
each testing sample. The mixing time was estimated. Therefore, the batch ticket obtained could
be different from the testing concrete.

3.2 Test Results

3.2.1 US 71 (Atlantic Project)

3.2.1.1 Batch Ticket

All batch tickets are listed in Appendix A. As mentioned before, these batch tickets may not be
the real batch tickets for the tested samples. However, these tickets still show that the concrete
mix is very consistent from time to time. Figure 4 shows the variation of the w/c ratio of all
mixes. There was little variation from mix to mix. The w/c ratio ranged from 0.389 to 0.436. The
mean value was 0.410 and the standard deviation was 0.016. One noticeable change of the
mixing tickets is the moisture content of aggregates. For the first two days, the moisture content
was 5.0%, 0.7%, and 1.5% for the fine, coarse, and intermediate aggregates, respectively. On the
last two days the moisture content for fine aggregate dropped to 0.6% and 0.2%. But the
moisture content for coarse aggregate increased to 4.9% and 4.2%. The value for the
intermediate aggregate was relatively constant, which was 1.4% and 1.0%. This means that the
moisture of aggregates changed during the project; it is every important to adjust the water used
in concrete mixture to get consistent concrete mix.

12
 0.44

0.43

0.42

w/c
0.41

0.40

0.39

0.38

Figure 4. Water to cement ratio for the mixes of US 71 (Atlantic project)

3.2.1.2 Concrete and Pavement Information

The concrete properties and pavement construction information are listed in Table 2. The
subbase temperature was tested at two locations. The results show that the temperature below the
surface is much lower than the temperature on the surface. The high temperature on the surface
could be caused by the radiation of the sun. The difference between the two subbase temperature
measurements ranges from a couple degrees to over 20°F. Therefore, it is important to put the
temperature at the right place when this value is used for the modeling purpose. Concrete
temperature was varied from 78°F to 87°F. At noon, it was slightly higher than in the morning
and afternoon.

In the pavement construction, the paving was processed right after the concrete was placed in the
field, and it was followed by finishing and curing. There were only a couple minutes between the
finishing and curing. Since the construction process was very consistent for this project, the
finishing and curing times were only recorded for a couple days. For the rest of construction, we
assumed that the finishing and curing times were the same as before. The sawing time was
around 11 hours despite the paving time except for the last two tests on July, 20, 2007, which
were 8.4 and 8.7 hours from the mixing time. The air content of concrete ranged from 6% to
7.5%, which is in the range of the designed value. The slump was from 1.25 in. to 2.25 in. The
variation is only 1 in. The unit weight of concrete is between 140 and 150 lb/ft3.

13
 Table 7. Concrete and pavement information for US 71 (Atlantic project)
Set time
Subbase temp. Sawing time Unit
Mixing Concrete Dump Paving Finishing Curing Air Slump (ASTM)
Date weight
time Infrared Probe temp. (°F) time time time time % in. Initial Final
Time hr (lb/ft3)
(°F) (°F) (hr) (hr)
6/27/ 12:38 1:02 1:14 10:57
07 p.m. 121.2 97.9 86.7 p.m. p.m. 1:16 p.m. 2:12 p.m. p.m. 10.32 6.00 1.75 145 8.09 10.57
6/27/ 2:35 3:00 3:04 2:05
07 p.m. 103.1 89.1 85.1 p.m. p.m. 3:06 p.m. 3:51 p.m. a.m. 11.50 6.80 1.75 142 8.75 12.38
6/28/ 9:22 9:47 9:59 10:34 9:10
07 a.m. 89.9 79.2 81.7 a.m. a.m. 10:01 a.m. a.m. p.m. 11.80 7.50 0.75 143 8.14 10.65
6/28/ 11:16 11:41 11:47 12:23 10:03
07 a.m. 94.5 83.5 80.1 a.m. a.m. 11:49 a.m. p.m. p.m. 10.78 7.00 1.75 144 8.04 10.24
6/28/ 1:40 2:05 2:08 2:59
07 p.m. 95.5 92.0 82.6 p.m. p.m. 2:11 p.m. 2:54 p.m. a.m. 13.32 7.25 1.75 143 7.43 10.09
6/29/ 9:11 9:31 9:36 10:17
07 a.m. 93.6 75.6 78.1 a.m. a.m. 9:39 a.m. a.m. - - 7.50 1.63 144 7.80 10.50
6/29/ 10:59 11:19 11:26 12:10
07 a.m. 88.0 80.0 81.4 a.m. a.m. 11:29 a.m. p.m. - - 7.50 1.50 145 7.40 9.80

14
6/29/ 2:57 3:17 2:10
07 p.m. 103.5 90.0 81.0 p.m. - - - a.m. 11.22 7.00 1.50 145 7.30 9.40
6/30/ 8:52 9:12 7:30
07 a.m. 85.5 76.4 78.1 a.m. - - - p.m. 10.63 7.00 1.38 146 8.30 10.40
6/30/ 11:45 12:05 11:00
07 a.m. 109.5 95.2 80.4 p.m. - - - p.m. 11.25 7.60 1.50 148 7.00 10.00
6/30/ 1:23 1:43 12:49
07 p.m. 99.5 89.0 81.0 p.m. - - - p.m. 11.43 6.80 2.25 143 8.40 11.20
7/2/0 9:08 9:28 8:15
7 a.m. 89.5 82.4 80.2 a.m. - - - p.m. 11.12 7.60 1.50 145 8.90 11.60
7/2/0 10:34 10:54 9:00
7 a.m. 100.2 84.2 82.4 a.m. - - - p.m. 8.43 7.00 1.25 145 8.10 9.70
7/2/0 12:40 1:02 9:23
7 p.m. 116.0 102.0 86.5 p.m. - - - p.m. 8.72 6.80 1.38 146 6.50 8.70

14
3.2.1.3 AdiaCal Calorimeter Results

The ASTM C403 was performed for each test sample for initial and final set. In addition to the
ASTM method, the AdiaCal (Figure 5), which is a semi-adiabatic calorimeter, was also used to
test concrete temperature development history and set times. In order to differentiate the set
times from these two methods, the set times from AdiaCal is called AdiaCal thermal set time. In
phase II an AdiaCal calorimeter with 3 in. by 6 in. concrete cylinders was employed. After the
phase II study, WR Grace developed a better AdiaCal calorimeter, which uses 4 in. by 8 in.
concrete cylinders. In the phase III study, this new AdiaCal was used to monitor concrete
temperature and determine thermal set.

Figure 6 shows one typical test result from the AdiaCal. The calorimeter recorded concrete
temperature with time. There are two methods to determine the thermal set: derivatives and
fraction methods (5). In phase III, the fraction method was applied since it is more robust than
the derivatives method. The fraction number has to be calibrated from the ASTM set time tests
and kept constant for each mix. To run a calibration test, both the AdiaCal and ASTM tests use
the same mix. The setting times are determined from the ASTM C403 tests first. The fraction
numbers for AdiaCal tests are then determined based on the fact that the set times determined
from both methods should be equal. In this project, the first set of ASTM C43 and AdiaCal were
used to calibrate the fraction number. For the rest of the tests, the fraction numbers were kept
constant.

Figure 5. AdiaCal calorimeter

15
 Figure 6. AdiaCal test results and determination of the set times

Figure 7 shows the relationship between the ASTM set times and AdaiCal thermal set times. The
results from these two methods are not equal but all test points are all around the equality line.
The difference between these two methods is less than one hour except one point. The average
variation is 0.47 hours for initial set and 0.66 hours for final set. For the final set, there is one
point with a large difference of 2.08 hours. The variation could be from two aspects: error from
the ASTM test or testing error from the AdiaCal test. As stated in ASTM C403, the single-
operator coefficient of variation on each of three batches made on different days is 7.1% and
4.7% for the initial and final setting time, respectively. Therefore, the range of results obtained
on three separate batches by the same operator with the same apparatus, using the same materials
and temperature conditions, on three different days should not exceed 23% of their average for
initial set time and 16% for final set time. The difference between these two tests was less than
23% percent of ASTM test for initial set. The highest difference is 10.2% and the average is
6.3%. For the final set time, the difference is less than 16% except one point. The highest
difference is 16.8% and the average is 6.2%.

Like the other test, the AdiaCal tests conducted in this field project also showed quite large
variation as shown in Figure 7. The variation could come from at least three sources: (1)
variation due to the equipment and test procedure, (2) variation in the environmental
temperature, which was different for the tests done at different times, and (3) the variation due to
the fraction selected for thermal set time prediction. In this project, the fraction number was
determined only based on one set of field tests because of the busy field test schedule. Much
smaller variations in the relationship between the AdiaCal thermal set times and ASTM set times
were found in the tests of the other two field projects (Alma Center, WI and Ottumwa, IA).

16
 10

Initial Set Time

Adia Cal Thermal Set Time (hour)

9

6
6 7 8 9 10

ASTM Set Time (hour)

(a) Initial set

13

Final Set Time

12
AdiaCal Thermal Set Time (hour)

11

10

8
8 9 10 11 12 13

ASTM Set Time (hour)

(b) Final set

Figure 7. ASTM set time vs. AdiaCal thermal set time from US 71 (Atlantic, IA) field study
(Initial thermal set—17% and 14% fraction for two AdiaCal, respectively; Final thermal
set—50% fraction for both AdiaCal)

3.2.1.4 Isothermal Calorimeter Results

The isothermal calorimeter, which was studied in phase II, was carried to the field. For each day,
one test was performed due to the duration of the testing time. In phase II only mortar samples
were tested. In the field both concrete and mortar samples were tested. For each test, four mortar
samples and four concrete samples were tested. Figures 8 and 9 show the isothermal calorimetry
results from different days using mortar and concrete samples.

During the first couple hours, the rate of heat evolution was negative. This was caused by sample
stabilization. Since sample temperature was lower than the temperature of calorimetry, the
samples absorbed heat from the calorimeters. Therefore the rate of heat evolution was negative.
The unit of heat evolution was calculated in term of per gram cementitious materials.

17
Figures 8 and 9 show that all the hydration curves have similar shapes with two hydration peaks.
There is little variation in the values of the second peak. The time for the peak value was slightly
delayed for the test on July 2nd. Compared with the mortar sample, concrete has lower peak
values. This could be caused by the sieving and the size of concrete sample. When the mortar
was sieved from concrete, part of the mortar was left with coarse aggregate. The sieved mortar
could be slightly different from the original mortar in concrete. Also, the concrete samples were
only 300 g; it was hard to get a representative concrete sample. It was easy to get more aggregate
or paste in the sample compared with the designed value. All these factors could cause the
difference between the mortar and concrete sample.

Figure 8. Isothermal calorimetry results for US 71 (Atlantic, IA) field mortar samples

Figure 9. Isothermal calorimetry results for US 71 (Atlantic, IA) field concrete samples

18
3.2.1.5 Semi-Adiabatic Calorimetry (IQ Drum) Test

Figure 13 shows the results from the semi-adiabatic calorimetry test. The main purpose of this
test is to provide the data for HIPERPAV analysis. After 120 hours, the generated heat was about
120 BTU/g cementitious materials. At the very beginning the heat evolution was slow. After a
couple hours, the generated heat started to increase quickly until 15 hours–20 hours. After that
the heat evolution increased much slower. Concrete hydrated slightly faster than mortar samples.
This could be caused by the higher temperature of concrete. The higher the temperature, the
faster the hydration occurred.

(a) Mortar sample

(b) Concrete sample

Figure 10. Heat evolution with time for US 71 (Atlantic, IA) field test

19
3.2.1.6 Maturity-Strength Results

Maturity and strength were tested for concrete samples until 28 days. The 4 in. by 8 in. cylinder
samples were casted and put into the curing tank inside the mobile lab. After getting back to ISU,
the samples were transferred into the curing room and cured until the test date. The temperature
of the curing tank inside the mobile lab was set at 70°F. One Ibutton was placed in the middle of
the sample to monitor concrete temperature. Maturity and strength were plotted in Figure 10.
There was a strong linear relationship between strength and maturity. The R-square value is 0.99.
The 28-day strength is almost 5000 psi.

Figure 11. Maturity-strength relationship for US 71 (Atlantic, IA) samples

3.2.1.7 Pavement Temperature

During the pavement construction, several Ibuttons were put inside the slab after measuring
concrete temperature development. On June 27th and 30th, a stick with three Ibuttons was inserted
into the pavement. The first Ibutton was one inch below the surface, the second one was in the
middle, and the third one was one inch above the bottom. The stick was placed one foot from the
edge of the pavement to avoid the edge effect due to heat exchange between slab and
environment. The temperature profiles were shown in Figure 11. For both tests, the top
temperature was more affected by the environment since it was close to the surface. It was higher
at day time and lower at night time. In Figure 11(a) the bottom temperature was missing due to
an equipment issue. The first peak of middle pavement temperature on July 27th was about 5°C
higher than that of July 30th. This could be caused by the higher concrete placement temperature,
which will accelerate cement hydration.

Figure 12 shows the temperature in the middle of the pavement tested at different days. The
difference among these results should be caused by the environment conditions, the time of
placement, and cement hydrations.

20
 (a) Temperature measured on July 27th

(b) Temperature measured on July 30th

Figure 12. Pavement temperature from US 71 (Atlantic, IA) field tests

21
 Figure 13. Pavement temperature from US 71 (Atlantic, IA) measured at the middle on
different date

3.2.2 HW 95 (Alma Center Project)

3.2.2.1 Batch Ticket

All 12 batch tickets are listed in Appendix B. The w/c ratios are consistent and close to the
designed value for all mixes expect one mixed at 10:51 a.m., July 17th, which had higher cement
content and a lower w/c of 0.392. The purpose of this mix was to provide high early-age strength
because the slab that was paved in the afternoon had to be opened to traffic the next day. The
results of other tests clearly showed the difference between this mix and others. The rest of the
w/c ratios were plotted in Figure 14. All w/c ratios were between 0.44 and 0.44. The average
value was 0.45. The standard deviation was 0.004.

0.47

0.46
w/c

0.45

0.44

0.43

Figure 14. Water to cement ratio for the mixes of HW 95 (Alma Center, WI) project

22
3.2.2.2 Concrete and Pavement Information

For the Alma Center project, only three day tests were conducted. There were four round tests
for each, two in the morning and two in the afternoon. The concrete and construction information
are listed in Table 4. Again the subbase temperature measured by two methods was different.
The temperature measured by the probe underneath the surface was a couple degrees lower. The
surface temperature ranges from 76°F to 115°F. Even in the same day the temperature difference
could be as much as 28°F. The concrete temperature was controlled around 75°F. The highest
temperature was 79.2°F and the lowest was 72.5°F. Concrete normally will be dumped in front
of the paver less than 10 minutes after mixing. The paving was carried out right after the
dumping. Then the finishing was applied. However, the curing for this project was delayed. It
was applied about 1 1/2 to 3 hours after the finishing. The slab was cut about 10 to 12 hours after
the mixing time, except for the last test. The sawing time for the last test was 16.8 hours: much
longer than the rest of the tests. This was caused by the environmental temperature, which was
between 40°F and 50°F during the night. The low temperature delays the strength development,
which in turn affects the saw cutting time. The properties of fresh concrete were close for all
different tests except the second test on the first day. This test showed low air content, w/c ratio,
slump, and setting time, but high unit weight. The air content ranged from 5.8% to 7.8%. The
slump was from 1 in. to 2.75 in. The unit weight was from 148 lb/ft3 to 154 lb/ft3. The initial set
happens after seven and before 10 hours. The final set times were from nine to 12 1/2 hours. The
w/c ratio was also determined from the microwave method. The determined w/c ratio ranges
from 0.4 to 0.47, which is close to the real w/c ratio.

23
 Table 8. Concrete and pavement information for HW 95 (Alma Center, WI) project
Set time
Subbase temp. Con. Sawing time Unit
Mixing Dump Paving Finishing Curing Air Slump (ASTM) Microwave
Date temp. weight
time Infrared Probe time time time time (%) (inch) Initial Final w/c
(°F) Time Hr (lb/ft3)
(°F) (°F) (hr) (hr)
7/17/0 8:32 8:42 8:50 10:31 8:05
7 a.m. 76.1 75.2 73.1 a.m. a.m. 8:53 a.m. a.m. p.m. 11.38 5.8 2.00 150 8.89 11.36 0.47
7/17/0 10:52 11:00 11:10 11:12 12:36 10:30
7 a.m. 91.2 88.0 73.9 a.m. a.m. a.m. p.m. p.m. 11.63 4.0 0.75 154 4.74 5.91 0.39
7/17/0 1:28 1:32 1:37 4:30 1:40
7 p.m. 92.0 88.3 75.0 p.m. p.m. 1:40 p.m. p.m. a.m. 12.20 7.0 1.00 154 7.45 9.61 0.44
7/17/0 2:59 3:02 3:07 4:47 3:00
7 p.m. 100.0 96.4 79.2 p.m. p.m. 3:09 p.m. p.m. a.m. 11.98 6.5 1.75 150 7.01 9.05 0.41
7/18/0 9:23 9:27 9:31 12:11 7:40
7 a.m. 88.7 82.6 74.7 a.m. a.m. 9:33 a.m. a.m. p.m. 10.28 7.5 2.75 148 7.98 10.31 0.45
7/18/0 10:47 10:52 10:59 11:01 12:20 9:15

24
7 a.m. 103.9 98.6 75.0 a.m. a.m. a.m. a.m. p.m. 10.47 5.8 1.25 153 7.72 10.00 0.46
7/18/0 2:07 2:11 2:15 3:40 1:25
7 p.m. 105.6 103.1 77.7 p.m. p.m. 2:17 p.m. p.m. a.m. 11.30 7.8 2.25 148 7.79 10.23 0.38
7/18/0 3:08 2:30
7 p.m. - - - - - - - a.m. 11.37 7.3 1.50 150 8.01 10.70 0.41
7/19/0 8:59 9:08 9:19 10:33 8:20
7 a.m. 87.0 81.9 72.5 a.m. a.m. 9:23 a.m. a.m. p.m. 11.52 6.0 1.50 151 9.11 11.48 0.41
7/19/0 10:31 10:37 10:42 10:44 12:25 9:20
7 a.m. 92.8 92.7 73.2 a.m. a.m. a.m. p.m. p.m. 10.82 6.0 1.50 151 8.65 11.18 0.40
7/19/0 11:54 12:04 11:50
7 a.m. 104.3 73.2 p.m. - - - p.m. 11.93 6.5 2.00 150 9.71 12.39 0.42
7/19/0 1:55 2:05 6:45
7 p.m. 114.9 105.3 74.7 p.m. - - - a.m. 16.83 7.5 1.25 152 9.08 12.06 0.40

24
3.2.2.4 AdiaCal Calorimetry Results

AdiCal calorimeter was also used to determine the thermal set time in this project. As stated in
the Atlantic project, the ASTM set time method will have variation even for the same operator
and materials. In order to reduce the error caused by the operation,in this project, two tests were
conducted for each testing concrete. The average value was used to compare with the results
from the AdiaCal test. Figure 15 shows the setting times determined from the ASTM and
AdiaCal methods. Most of the pints are on or very close to the equality line. The largest
difference is 1.8 hours for the initial set and 1.2 hours for the final set. The average differences
are 0.5 hours and 0.4 hours for the initial and final set time, respectively. The difference was less
than 23% of the ASTM test for initial set. The highest difference is 18.2% and the average is
6.1%. For the final set time, the difference is less than 16% except one point. The highest
difference is only 8.1% and the average is 3.7%.The results indicate the AdiaCal calorimeter is
able to estimate the set time for the field concrete. Like the Atlantic project, the fraction numbers
were determined from the first set of ASTM and AdiaCal tests. And the values were kept the
same for the rest of the tests.

One of the other purposes of the AdiaCal test is to check if this equipment could be used to
identify the changes of concrete mix or construction. Figure 16 shows the temperature curves
from four different tests conducted in the same day. Each test had two samples. A total of eight
samples were tested. It can be seen that the concrete samples from different batches had different
temperature histories. Even for the two tests from the same batch, the temperature could have
some difference. The temperature will be influenced by the initial temperature and also the
environment. Therefore, it is hard to use concrete temperature from AdiaCal tests as daily quality
control tools.

25
 12
Initial Set
10

AdiaCal Thermal Set Time (hr)

8

0
0 2 4 6 8 10 12

ASTM Set Time (hr)

(a) Initial set time

14

12
AdiaCal Thermal Set Time (hr)

10

0
0 5 10 15
ASTM Initial Set Time (hr)

(b) Final set time

Figure 15. ASTM set time vs. AdiaCal thermal set for HW 95 (Alma Center, WI) project,
18% fraction for initial thermal set and 41% for final thermal set

26
 37

35

33
Temperature (°C)

31

29

Test 1-1 Test 1-2

27 Test 2-1 Test 2-2
Test 3-1 Test 3-2
Test 4-1 Test 4-2
25
0 6 12 18 24

Time

Figure 16. Temperature from AdiaCal tests (tests were performed on HW 95, July 18th)

3.2.2.5 Isothermal Calorimetry Results

Three isothermal calorimetry tests were performed on mortar and concrete for this project. The
heat evolution curves have the similar trend for both mortar and concrete samples. The test on
July 19th had the lowest value and the test on July 17th had the highest values for both mortar and
concrete samples. Tests on July 17th and 18th had very similar peak values. But the peak time for
the 18th test was slightly longer. The difference is less than one hour. Compared with the results
from mortar samples, concrete samples have lower values. Despite these differences, the results
show that for the similar field concrete, the calorimetry results are similar. Therefore, it is
possible to use this simple isothermal calorimeter for daily quality control.

27
 (a) mortar sample

(b) concrete sample

Figure 17. Isothermal calorimetry results from HW 95 (Alma Center, WI) field study

3.2.2.6 Semi-Adiabatic Calorimetry (IQ Drum) Test

Figure 20 shows the IQ drum test results for mortar and concrete samples. The generated heat
was about 130 BTU/lb after 150 hours of hydration. For concrete sample, the rate of heat
evolution was reduced after about 50 hours. Compared with mortar sample, concrete generated
more heat at an early age.

28
 (a) Mortar sample

(b) Concrete sample

Figure 18. Heat evolution with time for HW 95 (Alma Center, WI) project field test

3.2.2.7 Maturity-Strength Results

The compressive strength was tested at 1, 3, 7, 14 and 28 days. One Ibutton was placed in the
middle of one concrete sample. However, the Ibutton was broken. The temperature data was not
available for this project. Since all the samples were cured in the curing tank inside the mobile

29
lab and also the curing room, it is assumed that the temperature of samples was constant. The 28-
day compressive strength is a little bit lower than 5000 psi.

Figure 19. Maturity-strength relationship for HW 95 (Alma Center, WI) samples

3.2.2.7 Pavement Temperature

The pavement temperature was measured at two locations each day on July 18th and 19th. The
top, middle, and bottom temperature was only measured in the morning July 18th. For the rest of
the tests, only the middle temperature was monitored. Figure 19 shows the results. The variation
of the top temperature was larger than middle and bottom due to the influence of the
environmental temperature. It was about 5°F higher at peak than the bottom temperature. For the
middle temperature, the highest was 100°F. Concrete casted on July 19th had lower temperature
compared with concrete on July 18th. The concrete casted in the morning of July 18th had the
highest first peak value.

30
 (a) Temperature at different depth

(b) Middle temperature measured at different date

Figure 20. Pavement temperature for HW 95 (Alma Center, WI) project

3.2.3 Ottumwa Project

3.2.3.2 Batch Ticket

All batch tickets were listed in Appendix 1. There were two tickets missing for July 24th tests due
to the printer problem. As shown in Figure 21, all mixes had a w/c ratio from 0.35 to 0.39, which
was a little bit lower than the designed value, 0.40. The average w/c ratio was 0.37. The standard
deviation was 0.01.The batch tickets show that the mixes at different times were consistent.

31
 0.39

0.39

0.38

0.38

w/c
0.37

0.37

0.36

0.36

0.35

Figure 21. Water to cement ratio for the mixes of US 63 bypass (Ottumwa, IA) project

3.2.3.3 Concrete and Pavement Information

The concrete and pavement information were summarized in Table 6. Pavement was cured about
30 min to one hour after finishing. The sawing time was shorter than the other two projects. It
was from 6.8 hours to 10 hours. The air content was from 5.8% to 7%, which was close to the
designed value of 6%. The slump was lower than the 2 in. designed values. The slump was from
1.0 in. to 1.5 in. Concrete unit weight was from 140 lb/ft3 to 146 lb/ft3. The setting times were
also shorter than the other projects. The initial setting time was around 4 hours and final setting
time was about 6 hours. The setting times are much shorter than for the other two projects. The
microwave w/c ratio was lower than the values from the batch tickets.

32
 Table 9. Concrete and pavement information for US 63 bypass (Ottumwa, IA) project

Set time
Subbase temp. Con. Sawing time Unit
Mix Dump Paving Finish Curing Air Slump (ASTM) Microwave
Date temp weight
time infrared probe time time time time (%) (inch) Initial Final w/c
(°F) Time hr (lb/ft3)
(°F) (°F) (hr) (hr)
7/24/ 8:30 8:34 8:43 8:51 9:45 4:00 6.0
80.0 74.3 80.6 7.50 1.00 144.1 4.38 6.89 0.363
07 a.m. a.m. a.m. a.m. a.m. p.m. 0
7/24/ 10:13 10:20 10:26 10:33 11:24 5:00 7.0
88.8 82.9 84.2 6.78 1.00 143.6 4.20 5.66 0.359
07 a.m. a.m. a.m. am a.m. p.m. 0
7/24/ 12:40 12:48 1:02 1:09 1:34 9:05 7.0
90.6 91.3 87.6 8.42 1.00 140.9 3.89 5.58 0.331
07 p.m. p.m p.m p.m p.m p.m. 0
7/24 2:26 2:33 2:39 2:50 3:19 10:30 6.7
91.9 95 88.0 8.07 1.00 140.6 3.97 5.50 0.309
/07 p.m p.m p.m p.m p.m p.m. 5
7/25/ 8:33 8:42 8:48 8:59 9:25 5:05 5.7
79.8 75.2 82.6 8.53 1.00 146.3 4.41 5.78 0.385
07 a.m. a.m. a.m. a.m. a.m. p.m 5
7/25/ 9:58 10:03 6:38 6.7
90.1 84.9 83.5 8.67 1.00 144.2 4.05 5.33 0.378
07 a.m. a.m. - - - p.m 5
7/25/ 12:30 12:39 12:46 12:55 1:31 9:38 7.0
96.1 93.7 88.5 9.13 1.25 144.5 3.86 5.31 0.34

33
07 p.m p.m p.m p.m p.m p.m 0
7/25/ 1:56 2:05 12:00 7.1
101.5 98.2 88.5 10.07 1.00 144.0 3.72 5.17 0.376
07 p.m p.m - - - p.m 0
7/30/ 8:16 8:25 6.7
79.2 75.9 83.1 1.00 143.7 4.68 6.55 0.35
07 a.m. a.m. - - - - - 5
7/30/ 9:32 9:47 7.7
90.3 81.7 81.3 1.50 141.0 4.55 6.37 0.318
07 a.m. a.m. - - - - - 5
7/30/ 1:37 1:50 7.5
97.3 91.6 85.5 1.25 142.2 4.54 6.39 0.319
07 p.m p.m - - - - - 0
7/30/ 3:15 3:23 6.7
101.9 96.3 88.2 1.00 144.7 4.55 6.44 0.356
07 p.m p.m - - - - - 5
7/31/ 8:47 8:57 6.0
84.2 77.5 82.4 1.00 145.4 4.32 5.84 0.367
07 a.m. a.m. - - - - - 0
7/31/ 10:51 11:01
94.3 81 84.6 145.4 4.38 6.08 0.356
07 a.m. a.m. - - - - - - -

33
3.2.3.4 AdiaCal Calorimetry Results

Fourteen AdiaCal tests were performed. The fraction numbers are 13% and 49% for
initial and final thermal set, respectively. These fraction numbers were determined from
the first set test. Similar to the other two projects, the setting time determined from these
two methods is very close. The largest difference is only 0.72 hours for both initial and
final setting time. The average difference between the ASTM and AdiaCal is 0.13 hours
and 0.23 hours for the initial and final setting times, respectively.
5
Initial Set
AdiaCal Thermal Set Time (hr)

4.5

3.5

3
3 3.5 4 4.5 5

ASTM Set Time (hr)

(a) Initial set time

8
Final Set
AdiaCal Thermal Set Time (hr)

4
4 5 6 7 8
ASTM Set Time (hr)

(b) Final set time

Figure 22. ASTM set time vs. AdiaCal thermal set for US 63 bypass (Ottumwa, IA)
project—13% fraction for initial thermal set and 49% for final thermal set

34
3.2.3.5 Isothermal Calorimetry Results

Figure 23 shows the isothermal calorimetry results. The test on July 31st shows earlier
hydration than other tests. The peak is about one hour earlier. The other three tests had
almost the same rate of hydration at the early time. However, the peak values were
different for these tests. Both concrete and mortar have the similar trend.

35
 7

Mortar 7/24
6
Mortar 7/25

mortar 7/30
Rate of Heat Evolution (mW/g)
5
mortar 7/31
4

0
0 3 6 9 12 15 18 21
Time (hour)

(a) Mortar sample

7

Concrete 7/24
6
Concrete 7/25
concrete 7/30
5
concrete 7/31
Rate of Heat Evolution (mW/g)

0
0 3 6 9 12 15 18 21
Time (hour)

(b) Concrete sample

Figure 23. Isothermal calorimetry results for US 63 bypass (Ottumwa, IA) project

36
3.2.3.6 Semi-Adiabatic Calorimetry (IQ Drum) Test

Figure 25 shows the IQ drum test results. The concrete sample hydrated faster at early
age due to the higher temperature. The highest concrete temperature during the test was
113.7°F. For mortar sample, the highest temperature was only 86.4°F. The difference was
almost 30°F. The generated heat was about 140 BTU/lb at 150 hours for concrete sample
and 120 BTU/lb for mortar samples at 200 hours. After about 40 hours, the hydration of
concrete samples slowed down.

(a) Mortar sample

(b) Concrete sample

Figure 24. Heat evolution with time for US 63 bypass (Alma Center, WI) project

37
3.2.3.7 Pavement Temperature

Figure 24 shows the pavement temperature tested on two different days. The Ibuttons
were put into the pavement around noon. The temperature difference inside pavement is
about 7°F at peak time. On the first day, the middle layer had the highest temperature due
to cement hydration and less heat loss. The first peak value was reached around 6 p.m..

(a) Temperature at different depth

(b) Middle temperature measured on July 25th

Figure 25. Pavement temperature for US 63 bypass (Ottumwa, IA) project

38
3.3 Comparison of Field Test Results from Different Projects

3.3.1 AdiaCal Calorimeter

As shown in each project, the thermal set time determined from the AdiaCal calorimeter
was close to the ASTM setting time. The data for all three projects are plotted in Figures
26 and 27. The initial ASTM setting time for different mixes ranges from 4 hours to 10
hours. The maximum difference between these two methods is only 1.77 hours, which is
about 18.2% of ASTM result. But the average variation is only 0.37 hours and the
standard deviation is 0.40. The variation is relatively larger for samples with long initial
set time.

12
AdiaCal Initial Thermal Set Time (hr)

10

0
0 2 4 6 8 10 12
ASTM Initial Setting Time (hr)

Figure 26. ASTM set time vs. AdiaCal thermal set time—initial set

Figure 27 shows the results of final setting time, it ranges from 5 to 13 hours. All the
points are distributed around the equality line. The maximum difference between these
two methods is only 2.08 hours, which is about 16.8% of ASTM result. But the average
variation is only 0.43 hours and the standard deviation is 0.45.

Since the tested initial and final setting times cover a large range and tests were
performed for different concrete mixes at different times, it can be concluded from the
results that the AdiaCal calorimeter could be used in the field to estimate concrete setting
time. Compared with ASTM test, the AdiaCal method is less labor-intensive especially
for samples with long setting times and could reduce the errors caused by operators.

39
 14

AdiaCal Final Thermal Set Time (hr)

12

10

0
0 2 4 6 8 10 12 14
ASTM Final Setting Time (hr)

Figure 27. ASTM set time vs. AdiaCal thermal set time—final set

As shown in Figure 16, samples casted in the same day had different temperature history.
Both the peak value and time to reach the peak could be different. More figures are listed
in the appendix. One of the reasons for the difference is the placement temperature. The
variation could be 5°C for the same project. This in turn will affect the hydration process
of cementitious materials. Another reason for the difference could be the environmental
temperature change. Even the samples were stored in a mobile lab where there is still
some room temperature variation. Also, AdiaCal is a simple semi-adiabatic calorimeter
with a relatively large coefficient of heat loss. All these factors can significantly affect
sample temperature history. At this stage, the concrete temperature is recommended for
daily quality control. However, if the placement and environmental temperature could be
controlled, this could be a possible method for quality control.

3.3.2 Isothermal Calorimeter

Figure 28 summarizes the isothermal calorimeter test results. The average value of each
project is used. It indicates that the results for mortar and concrete samples are not
identical. Concrete samples have lower peak values for the Atlantic and Alma Center
project but higher values for the Ottumwa project. As explained before, this could be
caused by the sampling issues. The peak time is slightly delayed for concrete samples.
This is possibly caused by the size of the sample. The concrete sample is about 300 g and
the mortar sample is only 100 g. For the concrete sample, the generated heat may take a
little longer to dissipate to the heat sink. It could delay the hydration curve.

40
 Figure 28. Summary of isothermal field calorimetry results

As shown in Figures 8, 17, and 23, for each project, the isothermal calorimeter results are
consistent for samples in different days. But, in order to use the simple isothermal
calorimeter for daily quality control,the calorimeter should also be able to detect the
difference when there is change in materials or other factors. Figure 28 shows the ability
of the isothermal calorimeter to detect the difference caused by materials and other
factors. In the figure, the three curves are different in terms of the shape and value. The
Ottumwa and Atlantic project had similar mix proportions but different cementitious
materials. The two calorimetry curves for these two projects are totally different.
Therefore, it is possible for the calorimeter to discover the change when the field mix is
changed.

3.3.3 Pavement Sawing Time

Figure 29 shows the pavement sawing time and AdiaCal final thermal set time. Most
concrete sawing times were between 6 and 14 hours after mixing. There is no clear
relationship between these two parameters. The sawing times are normally longer than
the set times. But some of them are every close.

41
 18

16

14

12

Sawing Time (hr)

10

0
0 2 4 6 8 10 12 14 16 18
AdiaCal Final Thermal Set Time (hr)

Figure 29. Pavement sawing time vs. AdiaCal thermal final set time

42
4. LAB TESTS FOR FIELD CONCRETE MATERIALS

Robust tests were conducted in lab for the concrete materials collected from the above-
mentioned three field sites: (1) US 71 PCC overlay, Atlantic, Cass County, Iowa, (2)
Highway 95, Alma Center, Jackson Country, Wisconsin, and (3) US 63 bypass,
Ottumwa, Wapello County, Iowa. Nine robust mixes, with 50% decrease/increase of WR
and/or FA dosages were developed based on the mix proportion actually used in field for
each field project. By changing the amount of FA and WR at a 50% level, robust tests are
used to simulate possible concrete mix proportion error that sometimes occurs in field
construction. The specific objectives of the robust tests are the following:
• To study the potential effects of over-doses or under-doses of WR and/or FA on heat
generation of concrete
• To find out whether or not the mixtures are acceptable or may have incompatibility
problems, the over- or under-dosed materials were used.
• To provide field engineers with acceptable boundaries to evaluate their calorimetry
test results, thus, calorimetry technology may be easily used as a tool for field
concrete quality control

AdiaCal tests were performed for each robust mix, and isothermal calorimeter tests were
performed for each robust mix at four different temperatures. Selected IQ drum tests and
ASTM C403 set time tests were also performed in lab so as to compare the lab results
with the field test results.

4.1 Tests and Methods

The following tests were conducted for materials and robust mixes of each field site:

1. Specific gravity and absorption of aggregates

2. AdiaCal calorimetry tests
3. Simple isothermal calorimetry test at 10oC (5oC for Alma Center, WI,
mixes), 20oC, 30oC, and 40oC
4. IQ Drum calorimetry tests
5. ASTM set time robust tests (for US 63 bypass, Ottumwa, IA, mixes only)

The aggregates of all three field projects were tested for specific gravity and absorption
according to ASTM C127 “Standard Test Method for Density, Relative Density (Specific
Gravity), and Absorption of Coarse Aggregate” and C128 “Standard Test Method for
Density, Relative Density (Specific Gravity), and Absorption of Fine Aggregate.”

The nine robust mixtures prepared using the materials from each field project are the
following:
Mix 1: A reference mix made with the same proportion as used in the field project
Mix 2: Mix 1 with over-dosed WR (50% more than that used in Mix 1)
Mix 3: Mix 1 with under-dosed WR (50% less than that used in Mix 1)
Mix 4: Mix 1 with over-dosed FA (50% more than that used in Mix 1)
Mix 5: Mix 1 with under-dosed FA (50% less than that used in Mix 1)

43
Mix 6: Mix 1 with over-dosed WR and FA (both WR and FA are 50% more than those
used in Mix 1)
Mix 7: Mix 1 with over-dosed WR (50% more than that used in Mix 1) and under-dosed
FA (50% less than those used in Mix 1)
Mix 8: Mix 1 with under-dosed WR (50% less than that used in Mix 1) and over-dosed
FA (50% more than that used in Mix 1)
Mix 9: Mix 1 with under-dosed WR and FA (both WR and FA are 50% less than those
used in Mix 1)

The robust mixture proportions of the three projects studied are presented in Tables 10–
12. The concrete (Mix 1) of all three field projects contained WR and 20% FA
replacement.

Table 10. Concrete mix proportions for US 71 project (Atlantic, IA)

Cement Fly ash C. Agg. Int. Agg. Sand Water AEA (fl WR (fl
Mix (pcy) (pcy) (pcy) (pcy) (pcy) (pcy) oz/cwt) oz/cwt)
1 442 110 1560 273 1309 221 0.3 4.0
2 442 110 1560 273 1309 221 0.3 6.0
3 442 110 1560 273 1309 221 0.3 2.0
4 383 170 1560 273 1309 221 0.3 4.0
5 497 55 1560 273 1309 221 0.3 4.0
6 387 165 1560 273 1309 221 0.3 6.0
7 497 55 1560 273 1309 221 0.3 6.0
8 387 165 1560 273 1309 221 0.3 2.0
9 497 55 1560 273 1309 221 0.3 2.0

Table 11. Concrete mix proportions for the HW95 project (Alma Center, WI)
Cement Fly ash C. Agg. Int. Agg. Sand Water AEA (fl WR (fl
Mix (pcy) (pcy) (pcy) (pcy) (pcy) (pcy) oz/cwt) oz/cwt)
1 446 113 1825 0 1370 252 1.0 3.2
2 446 113 1825 0 1370 252 1.0 4.8
3 446 113 1825 0 1370 252 1.0 1.6
4 390 170 1825 0 1370 252 1.0 3.2
5 503 57 1825 0 1370 252 1.0 3.2
6 390 170 1825 0 1370 252 1.0 4.8
7 503 57 1825 0 1370 252 1.0 4.8
8 390 170 1825 0 1370 252 1.0 1.6
9 503 57 1825 0 1370 252 1.0 1.6

44
Table 12. Concrete mix proportions for US 63 bypass project (Ottumwa. IA)
Cement Fly ash C. Agg. Int. Agg. Sand Water AEA (fl WR (fl
Mix (pcy) (pcy) (pcy) (pcy) (pcy) (pcy) oz/cwt) oz/cwt)
1 443 111 1846 0 1291 222 0.3 4.0
2 443 111 1846 0 1291 222 0.3 6.0
3 443 111 1846 0 1291 222 0.3 2.0
4 385 170 1846 0 1291 222 0.3 4.0
5 499 56 1846 0 1291 222 0.3 4.0
6 388 167 1846 0 1291 222 0.3 6.0
7 499 56 1846 0 1291 222 0.3 6.0
8 388 167 1846 0 1291 222 0.3 2.0
9 499 56 1846 0 1291 222 0.3 2.0

4 in. by 8 in. concrete cylinder samples were used for AdiaCal calorimetry tests. In the
test, all concrete mixtures were mixed according to ASTM C192 “Practice for Making
and Curing Concrete Test Specimens in the Laboratory.” The cylinder samples were then
prepared according to ASTM C192, and placed into the AdiaCal calorimeter right after
casting. After the samples were placed into the calorimeter, the pre-programmed
calorimeter started recording the concrete temperature immediately. The concrete
temperature was recorded every 1/2 min by the sensor located below the bottom of the
sample holder; the data was retrieved from the data logger through the program after 48
hours. The average values from at least two samples of each mix were used for analysis.
A total of 27 mixes were tested with AdiaCal calorimeter.

The isothermal calorimetry tests were done according to the procedures described in the
draft of the specification developed in phase II (Appendix E). Mortar samples were used
in the tests. Four different placement and test temperatures (10oC [or 5oC], 20oC, 30oC,
and 40oC) were selected for the tests. To control the concrete placement temperature, the
raw concrete materials from the three projects were first stored in a refrigerator, oven, or
room prior to mixing. Mortars were then mixed according to ASTM C305 “Standard
Practice for Mechanical Mixing of Hydraulic Cement Pastes and Mortars for Plastic
Consistency.” Four samples, with weights of 100+2 g each, were placed into standard
plastic containers and then loaded into the calorimeter immediately after samples were
ready. After the samples were placed into the calorimeter, the pre-programmed
calorimeter started taking readings immediately. The readings were taken every 1/2 min
for 72, 48, or 24 hours, depending upon the testing temperature. The rates of heat
evolution per g of cement were then calculated from the mix design of mortar, and the
average values from four samples of each mix were used for analysis. A total of 108
mixtures were tested with isothermal calorimeter at four different temperatures.
Semi-adiabatic calorimetry tests were conducted using IQ Drum for 6 in. by 12 in.
concrete cylinders. Only the reference mixes (Mix 1 in Tables 10–12) of each field
project were tested. The concrete was mixed according to ASTM C192 “Practice for
Making and Curing Concrete Test Specimens in the Laboratory.” The cylinder samples
were prepared according to ASTM C192, and placed into the calorimeter immediately
after casting. After the samples were placed into the calorimeter, the pre-programmed

45
calorimeter started taking readings immediately. The concrete mix proportion and
physical properties of the raw materials were input into the program, which provided the
desired results including the thermal history and heat evolution process of concrete. The
readings were taken every 15 min through the program, and the entire test took
approximately 7 days.

In phase II of the present project, investigators demonstrated that there was a close
relationship between the thermal setting values obtained from calorimetry tests and those
from the ASTM set time tests. In order to compare the concrete set times measured from
the two different methods, standard ASTM set time tests were also performed in the
phase III study in addition to the calorimetry tests. The standard ASTM tests were done
based on ASTM C403 “Standard Test Method for Time of Setting of Concrete Mixtures
by Penetration Resistance.” Only nine mortar mixes of the US 63 bypass (Ottumwa, IA)
project (Table 12) were selected and tested. The mortars were mixed according to ASTM
C305 “Standard Practice for Mechanical Mixing of Hydraulic Cement Pastes and Mortars
for Plastic Consistency.” The samples were placed and tested at room temperature until
final set were achieved.

4.2 Results and Discussion

4.2.1 US 71 Atlantic (IA) Project Mixes

4.2.1.1 AdiaCal Tests

Based on research from phase II, heat indexes were established to help engineers interpret
the calorimeter results, and predict concrete performance so as to be used for concrete
quality control. The heat indexes include thermal initial set and final set times, which are
determined from the first derivative of the temperature curves. The initial thermal set
time is defined as the time when the first derivative curve reaches its highest value, at
which point the increase in the sample temperature is the fastest. After the initial set time,
the first derivative values start to decrease. The final thermal set time is defined as the
time when the first derivative becomes zero, which corresponds to the time when the
highest sample temperature is achieved in the original temperature curve. In addition to
the thermal set times, the areas under the temperature curve during different test periods
are used (see Appendix E, Areas A, B, C, D, X, and Y represent the heat generated
during the first–sixth hours, sixth–12th hours, 12th–18th hours, 18th–24th hours, first–
24th hours [first day], and first–48th hours [first two days], respectively.) The data of the
first hour was not used in consideration that the calorimeter system needed a certain time
to reach its equilibrium status after samples were placed.

The temperature curves of concrete made with materials collected from the US 71,
Atlantic, IA, project and with nine different mix proportions (as shown in Table 10) are
shown in Figure 30. All calorimetry curves, from the mixtures with different WR dosages
and FA replacement levels and under different temperatures, displayed major peaks that
cover a certain area under the peaks, which indicates that there is no incompatibility
problem in the concrete mixtures in the ranges of WR and FA applied.

46
 Figure 30. AdiaCal robust test results of US 71 (Atlantic, IA) concrete mixes

The initial and final thermal set times from the original field mix (as shown in the
columns in the figure) and the maximum and minimum set times from the mixes with
different levels of WR and FA (as shown in the error bars in the figure) obtained from the
AdiaCal curves were summarized in Figure 31. The detailed thermal set times and areas
under heat generated curves at different periods of all nine mixes are listed in Table B.1..
The results showed that the initial thermal set times of the nine concrete mixtures tested
were between 9.5 hours and 19.7 hours, while the final thermal set times of the mixtures
were between 19.6 hours and 21.8 hours. The figure also shows that the variation of
initial thermal set time is larger than that of final thermal set time. In other words, the
amount of WR and/or FA has more impact on the initial set than on the final set of the
mixtures.

30
IS
FS
AdiaCal set time, hours

FS-IS
20

10

0
US71

Figure 31. Estimated set time from US 71 (Atlantic, IA) AdiaCal robust test

The areas under the temperature-time curves within different time periods were also

47
analyzed and the results (with the columns referring to the value from original field mixes
and the error bars referring to the maximum and minimum values from mixes with
different levels of WR and FA) are shown in Figure 32. The figure illustrates that the
areas under the calorimeter curves increased within the first 24 hours, which indicated
that more heat is generated through time in this period. Approximately the same amount
of heat was generated in the first and second day.

200 Area A (1-6h) 1250

Area B (6-12h)
Area C (12-18h)
1000 Area X (1day)
150 Area D (18-24h)
Area Y (2day)

Area, oFxh
Area, oFxh

750
100
500

50
250

0 0
US71 US71

Figure 32. Areas under AdiaCal test curves of US 71 (Atlantic, IA) project during
different test period

Statistical analysis was performed to study the effect of the amount of WR and FA
replacement on the initial and final thermal set time, the mortar setting window (FS-IS),
and peak temperature of AdiaCal tests. Least square fit was performed in the analysis of
these calorimeter test values. As shown in Figure 33, initial and final thermal set time
both increased with the level of WR and FA replacement. However, the effects of FA
replacements on these thermal parameters are more significant than that of WR. The
figure also suggests that the setting window (from initial setting to final setting time)
reduced with the increased FA replacement levels. The peak temperature from the
AdiaCal test reduced with the FA replacement; however, no obvious changes were found
with different water reducer dosage.

48
 20

Estimated, h

±0.765822
14.32217
16

IS-
12

8
22

Estimated, h
21.5

±0.392767
20.74444
21
FS- 20.5
20
19.5
11
9
±0.723767
6.411154
FS-IS, h

7
5
3
1
28.5
Temp, oC
27.45556
±0.58168

28
Peak

27.5
27
26.5
2
3
4
5
6

10
15
20
25
30
4
WR (fl 20.018
oz/cwt) SCMs/(c&SCMs)%

Figure 33. Statistical analysis from US 71 (Atlantic, IA) AdiaCal robust test

4.2.1.2 Isothermal Calorimetry Test Results

The heat evolution curves of the mortar used in the field concrete but tested at four
different temperatures (10oC, 20oC, 30oC, and 40oC) are shown in Figure 34. As seen in
the figure, similar to the results from the field isothermal calorimetry tests, all the heat
generation curves had two major peaks, which reflect FA replacement in the concrete
mixtures. These second peaks were not observed from the AdiaCal calorimetry test. With
increase in the testing temperature, the maximum rate of heat generation and the area
under the major peaks increases, while the times to reach this maximum rate also
decrease. This indicates that high curing temperature is favorable to the concrete strength
development, and extended curing time is needed for the concrete to gain a specific
strength value when concrete is under a low temperature environmental condition.

The initial thermal set time increased from 6.4 hours to 20.3 hours when the temperature
changed from 40oC to 10oC, while the final thermal set time increased from 9.3 hours to
29.4 hours when the temperature decreased from 40oC to 10oC.

49
Figure 34. Isothermal test results of US 71 (Atlantic, IA) Mix 1 at four temperatures

The heat generation curves of all nine different mixes for the US 71 Atlantic, Iowa,
project at four different temperatures (10oC, 20oC, 30oC, and 40oC) are shown in Figure
35. All calorimetry curves, from the mixtures with different WR dosages and FA
replacement levels and under different temperatures, displayed two major peaks that
cover a certain area under the peaks, which is related to FA effect. The similar shape of
the heat generation curves indicates that there is no incompatibility problem in the
concrete mixtures in the ranges of WR and FA applied.

The results showed that the initial thermal set times of the US 71 Atlantic, Iowa, mixtures
were between 20.3 hours and 28.8 hours at 10oC, between 12.2 hours and 19.5 hours at
20oC, between 7.2 hours and 15.5 hours at 30oC, and between 6.4 hours and 7.3 hours at
40oC. The final thermal set times were between 29.4 hours and 35.1 hours at 10oC,
between 17.5 hours and 28.6 hours at 20oC, between 10.7 hours and 16.1 hours at 30oC,
and between 9.3 hours and 10.0 hours at 40oC.

50
51
 Figure 35. Isothermal robust test results of US 71 (Atlantic, IA) mortar mixes at
different temperatures

The boundaries of initial and final thermal set time from the isothermal robust tests were
summarized in Figure 36. Similar to AdiaCal thermometry results, the columns refer to
the value from original field mixes and the error bars refer to the maximum and minimum
values from mixes with different levels of water reducer and fly ash. Results showed that
the initial and final thermal set times and the setting time window all increase with the
decrease of the environmental temperature. Also, the variations of the thermal set time
increase while the environmental temperature decrease. Unlike the AdiaCal test results,
the variation of the initial thermal set time appeared not clearly different from that of the
final thermal set times. The detailed thermal set times and the area under heat generation
curves at different time periods of each mixes can be found in Table C.1.–26.

40
US71 (Atlantic, IA)
Isothermal set time, hours

IS
30 FS
FS-IS

20

10

0
10oC 20oC 30oC 40oC
Testing temperature

Figure 36. Estimated set time from isothermal robust test on US 71 (Atlantic, IA) mixes

The areas under the heat generation time curves within different time periods were also
analyzed. Results in Figure 37 show that more heat was generated when the

52
environmental temperature was higher. At low temperature (10oC), the area increased
with the time elapse within the first 24 hours, which indicated more heat was generated.
The heat generation within 24 hours to 48 hours is higher than the first 24 hours after
cement makes contact with water. However, the heat generation will slow down after 48
hours. The larger area of the first hour to 6 hours might be caused by the stabilization
time of the sample, which will usually have a relatively high temperature compared to the
environmental temperature. With the increase of the environmental temperature, larger
amounts of heat were observed at an earlier period. The heat generation reaches the peak
at 6 hours to 12 hours, but slows down after 12 hours or 24 hours at 30oC and 40oC.
Results indicated high strength development at early ages when the environmental
temperature is higher.

40 80
Area A (1-6h) US71 (Atlantic, IA) US71 (Atlantic, IA))
Area B (6-12h)
30 Area C (12-18h) 60

Area, mWxh/g
Area, mWxh/g

Area D (18-24h)
20 40
Area X (1day)
10 20 Area Y (2day)
Area Z (3day)

0 0
10oC 20oC 30oC 40oC 10oC 20oC 30oC 40oC
Testing temperature Testing temperature

Figure 37. Heat generation from isothermal robust test mixes at different times US
71 (Atlantic, IA) mixes

Similar to the AdiaCal thermometry study, statistical analyses were performed in order to
study the effect of the amount of WR, FA replacement and environmental temperature on
the initial and final thermal set times and the peak heat generation rate in isothermal tests.
Least squares fit was performed on the prediction of initial thermal set (IS) and final
thermal set (FS), time between the final and initial sets, or set time window, (FS-IS), and
peak temperature from isothermal test using the parameters of WR dosage, FA
replacement % and environmental temperature. According to the results as shown in
Figure 38, both initial and final thermal set times decrease when the environmental
temperature goes up, the set time window (FS-IS) reduced with the increase of
environmental temperature. The initial setting and final setting time both increase with
the amount of WR used and the percent replacement of the FA. Environmental
temperature has most the significant effect on the initial setting and final thermal set
times and the peak heat generation rate. The set time window does not have obvious
changes with the increase of percentage replacement of FA and WR. FA replacement and
WR dosage do not have obvious effects on peak heat generation rate from the isothermal
test.

53
 30

±0.774774
12.36497
20

IS, h
15

5
±0.86133 35
17.5408

25
FS, h

15

5
12
±0.773176
5.176386
FS-IS, h

0
7
±0.239811
Peak Rate
3.35486

3
1
2
3
4
5
6

10
15
20
25
30
5

15
25

35
45
4 25
WR (fl 20.018 Env.
oz/cwt) SCMs/(c&SCMs)% Temp. (oC)

Figure 38. Effect of mix design and temperature on IS and FS from isothermal
robust test US 71 (Atlantic, IA mixes)

4.2.1.3 IQ Drum test results

The semi-adiabatic calorimetry (IQ Drum) test of the field mix was also performed in the
laboratory; the results of the heat generation curves will be used for the calculation of the
concrete performance with HIPERPAV program. Results obtained from the IQ Drum test
are shown in Figure 39. The results show that the heat evolution was slow at the first 5
hours, but it increased rapidly during 5 hours–20 hours and gradually became stable after
20 hours. The heat generated was about 120 BTU/gram cementitious materials at the time
of 150 hours, which was similar to that of the field IQ Drum test. This indicated a very
good consistency of the IQ Drum tests in the mobile lab and a conventional concrete lab.

54
 Figure 39. IQ drum test result of US 71 (Atlantic, IA) Mix 1

4.2.2 Alma Center (WI) Mixes

4.2.2.1 AdiaCal Test Results

AdiaCal calorimetry curves from all nine Alma Center (WI) mixes are shown in Figure
40. The thermal set times and the parameters related to the shape of the temperature
curves of each mix are given in Table 21.

Figure 40. AdiaCal robust test results of HW 95 (Alma Center, WI) mortar mixes

55
Similar to the US 71 (Atlantic, IA) project, all calorimetry curves, from the mixtures with
different WR dosages and FA replacement levels and under different temperatures,
displayed major peaks that cover a certain area under the peaks, which indicates that
there is no incompatibility problem in the concrete mixtures in the ranges of WR and FA
applied.

The results illustrate that the initial thermal set times are between 11.8 hours and 20.5
hours, while the final setting thermal set times are between 19.6 hours and 23.6 hours.
The initial and final thermal set times from the original field mix and the maximum and
minimum set times from the mixes with different levels of WR and FA obtained from the
AdiaCal curves were summarized in Figure 41. Similar to what observed in the US 71
Atlantic (IA) project, the variation of the initial thermal set times of these mixtures from
the AdiaCal tests is much larger than the variation of the final thermal set times. In other
words, the amount of WR and/or FA has more impact on the initial set than on the final
set of the mixtures.

30
IS
FS
AdiaCal set time, hours

FS-IS
20

10

0
HW95

Figure 41. Estimated set time from HW 95 (Alma Center, WI) AdiaCal robust test

The areas under the temperature-time curves within different time periods were also
analyzed and the results are shown in Figure 42. The figure illustrates that similar to the
results found in the US 71 project, the areas under the calorimeter curves increased
within the first 24 hours, which indicated that more heat is generated through time. Also,
approximately the same amount of heat was generated in the first and second day.

56
 200 1250

Area X (1day)
1000
150 Area Y (2day)

Area, oFxh
Area, oFxh

750
100
500
Area A (1-6h)
50 Area B (6-12h)
Area C (12-18h) 250
Area D (18-24h)
0 0
HW95 HW95

Figure 42. Areas under HW 95 (Alma Center, WI) AdiaCal test curves during
different test period

21
Estimated, h

19
±2.018203
15.28889

17
IS-

15
13
11
23.5
Estimated, h
21.04444
±1.00221

22.5
FS-

21.5
20.5
19.5
8
±1.353549
5.787778
FS-IS, h

2
29
±0.315992
Temp, oC
27.34444

28
Peak

27
26
2

5
10
15
20
25
30

3.22
WR (fl 20.2
oz/cwt) SCMs/(c&SCMs)%

Figure 43. Statistical analysis from the HW 95 (Alma Center, WI) AdiaCal robust
test

Statistical analyses were also performed to study the effect of the amount of WR and FA
replacement on the initial and final thermal set time, the mortar setting window (FS-IS),
and peak temperature of AdiaCal tests. As shown in Figure 43, initial and final thermal
set time both increase with the level of WR and FA replacement. The peak temperature

57
from the AdiaCal test reduced with the FA replacement and WR dosage. However, the
effects of FA replacements on these thermal parameters are more significant than that of
WR. The figure also suggests that the setting window reduced with the increased FA
replacement levels, while no obvious effects from WR were found. The peak temperature
from the AdiaCal test reduced with the FA replacement and WR dosage.

4.2.2.4 Isothermal Calorimetry Test

Isothermal calorimetry tests were performed at four different temperatures (5oC, 20oC,
30oC, and 40oC), where 5oC instead of 10oC was used in the study of Alma Center (WI)
mixes due to the weather conditions of the project location. Similar to what was used for
the US 71 Atlantic (IA) project, the rate of heat generation of the mortar was tested for 72
hours at the testing temperature of 5oC, 48 hours at the testing temperature of 20oC, and
24 hours at the testing temperatures of 30oC and 40oC. Figure 44 shows that the initial
thermal set times increased from 7.2 hours to 25.1 hours, while the final thermal set times
increased from 9.3 hours to 34.5 hours when the testing temperature dropped from 40oC
to 5oC.

Figure 44. Isothermal test results of HW 95 (Alma Center, WI) mortar mix 1 at
different temperatures

At the test temperature 20oC and above, all calorimetry curves, from the mixtures with
different WR dosages and FA replacement levels, displayed a regular calorimetry curve
shape and possess a certain peak height and width, which indicates that there is no
incompatibility problem in the concrete mixtures in the ranges of WR and FA applied.
However, the low heat generation at 5oC testing temperature might indicate prolonged set
time and potential construction problems.

The heat generation curves of all nine mixes of the Alma Center (WI) project tested at

58
four different temperatures (5oC, 20oC, 30oC, and 40oC) are shown in Figure 45. The
thermal set time and the area under heat generation curves at different time periods of
each mix are presented in Tables 27–30.

59
 Figure 45. Isothermal test results of HW 95 (Alma Center, WI) mortar mixes
different temperatures

The results show that the initial thermal set times of the Alma Center (WI) mixtures are
between 25.1 hours and 35.3 hours at 5oC, between 13.7 hours and 19.4 hours at 20oC,
between 11.8 hours and 14.2 hours at 30oC, and between 7.2 hours and 9.3 hours at 40oC.
The final thermal set times are between 34.5 hours and 45.0 hours at 5oC, between 20.5
hours and 25.1 hours at 20oC, between 15.0 hours and 15.8 hours at 30oC, and between
9.3 hours and 9.7 hours at 40oC. It is noted that at the low temperature (5oC), the initial
thermal set took place at approximately 24 hours, while the final thermal set can take
place at almost 40 hours. There is a little strength development of the mixture during the
first 72 hours after cast and cured at 5oC.

The boundaries of initial and final set from the isothermal robust tests were summarized
in Figure 46. Similar to the US 71 (Atlantic, IA) project, the initial and final thermal set
times and the setting time window all increased with the decrease of the environmental
temperature. The variation of the thermal set time values generally decreased with the
increased testing temperature. Also, unlike the AdiaCal test results, the variation of the

60
initial thermal set time appeared not clearly different from that of the final thermal set
times.

50
HW95 (Alma Center, WI)

Isothermal set time, hours

IS
40
FS
FS-IS
30

20

10

0
5oC 20oC 30oC 40oC
Testing temperature

Figure 46. Estimated set time from isothermal robust test on HW 95 (Alma Center,
WI) mixes

The areas under the heat-generation time curves within different time periods were also
analyzed, and results are shown in Figure 47. Similar to the US 71 project, more heat was
generated when the environmental temperature was higher. At low temperature (5oC), the
area increased with the time elapse within the first 24 hours, which indicated more heat
was generated. The heat generation within 24 to 48 hours is higher than the first 24 hours
after cement make contact with water. However, the heat generation will slow down after
48 hours. The larger area of the first 1–6 hours might be caused by the stabilization time
of the sample, which will usually have relatively high temperature compared to the
environmental temperature. With the increase of the environmental temperature, larger
amounts of heat were generated at an earlier period. Heat generation reaches the peak at 6
hours–12 hours, but slows down after 12 hours or 24 hours at 40oC. Results indicated
high strength development at early ages when the environmental temperature is higher.

50 80
Area A (1-6h) HW95 (Alma Center, WI)
HW95 (Alma Center, WI)
40 Area B (6-12h)
Area C (12-18h) 60
Area, mWxh/g

Area, mWxh/g

30 Area D (18-24h)
40
20
Area X (1day)
20 Area Y (2day)
10
Area Z (3day)

0 0
5oC 20oC 30oC 40oC 5oC 20oC 30oC 40oC
Testing temperature Testing temperature

Figure 47. Heat generation from isothermal robust test mixes at different times
HW95 (Alma Center, WI) mixes

61
Similar to the US 71 project, least squares fit was performed on the prediction of initial
thermal set (IS) and final thermal set (FS), setting time window (FS-IS) and peak
temperature from isothermal test using the parameters of WR dosage, FA replacement
percent, and environmental temperature. According to the results as shown in Figure 48,
both initial setting and final thermal set times decrease when the environmental
temperature goes up, and the setting time window (from initial setting to final setting
time) reduces with the increase of environmental temperature. The initial setting and final
setting time both increase with the amount of WR used and the percent replacement of
the FA. Environmental temperature has significant effect on the initial and final thermal
set times and the peak heat generation rate. FA replacement and WR dosage do not have
obvious effects on thermal set times and peak heat generation rate from the isothermal
tests on HW 95 (Alma Center, WI) mixes.

40
±0.873491

30
13.96813
IS, h

20
10
0
45
±1.133402
20.21086

35
FS, h

25
15
5
25
±1.333468
6.243284
FS-IS, h

15
10

0
8
±0.167676
Peak Rate

6
3.516077

4
2
0
2

5
10
15
20
25
30
0
10
20
30
40

3.22 23.75
WR (fl 20.215 Env.
oz/cwt) SCMs/(c&SCMs)% Temp. (oC)

Figure 48. Effect of mix design and temperature on IS and FS from isothermal
robust test HW 95 (Alma Center, WI) mixes

In addition to the above-mentioned robust tests, where a fixed low w/c of 0.45 was used,

62
a mortar sample with a w/c of 0.30 and over-dosed air entraining agent (AEA) and WR
approximately 6 times the original mixes were also studied using the isothermal
calorimeter at 30oC. A potential incompatibility problem was found with this mixture
(Figure 14, w/c=0.30) although it was not found in the previous robust tests (w/c=0.45).
As seen in Figure 49, the first major peak of heat generation rate was delayed from
approximately 12 hours to 24 hours when the w/c of the mixture decreased from 0.45 to
0.3 (with over-dosed AEA and WR). Another major hydration peak appeared at
approximately 60 hours after testing, thus considerably elongating the final set time and
strength development of the mixture.

Figure 49. Isothermal test results of mortar with normal and overdosed chemical
admixtures

4.2.2.5 IQ Drum Test Results

The semi-adiabatic calorimetry test results of the original Alma Center (WI) mix can be
found from the IQ Drum results as shown in Figure 50. Similar to the Atlantic (IA) mix,
results showed that the heat evolution was slow during the first couple hours; however,
the generated heat started to increase quickly after that until about 20 hours. The heat
generation rate was more stable after 20 hours. The generated heat was about 130 BTU/g
cementitious materials at 150 hours, which was quite similar to the results from the field
test. This indicated a very good consistency of the IQ Drum test.

63
 Figure 50. IQ Drum test result of the HW 95 (Alma Center, WI) concrete (Mix 1)

4.2.3 Ottumwa (IA) Mixes

4.2.3.1 AdiaCal test results

AdiaCal calorimeter was used to determine the thermal set time with the robust mix
design from the materials collected from Ottumwa (IA). The temperature curves from all
nine different mixes are shown in Figure 51, while the detailed information on the
AdiaCal thermal set time and the areas under the temperature curves of each mix can be
found in Table B.3..

64
 Figure 51. AdiaCal robust test results of US 63 bypass (Ottumwa, IA) concrete
mixes

Similar US 71 (Atlantic, IA) and HW 95 (Alma Center, WI) projects, all calorimetry
curves, from the mixtures with different WR dosages and FA replacement levels and
under different temperatures, displayed major peaks that cover a certain area under the
peaks, which indicate that there is no incompatibility problem in the concrete mixtures in
the ranges of WR and FA applied. Results showed that the initial thermal set times are
between 8.3 hours and 14.3 hours, while the final thermal set times are between 13.2
hours and 17.5 hours. The initial and final thermal set times from the original field mix
and the maximum and minimum set times from the mixes with different levels of WR
and FA obtained from the AdiaCal curves were summarized in Figure 52. The figure also
shows that the variation of initial thermal set time is larger than that of final thermal set
time. In other words, the amount of WR and/or FA has more impact on the initial set than
on the final set of the mixtures.

65
 30
IS
FS

AdiaCal set time, hours

FS-IS
20

10

0
US71 HW95 US63 bypass

Figure 52. Estimated set time from US 63 bypass (Ottumwa, IA) AdiaCal robust test

It can be observed in the figure that concrete made with US 63 bypass (Ottumwa, IA)
mix proportion and materials has early final setting time compared to concrete made with
the other two field mix designs and materials; however, there is no obvious difference on
the initial setting within three projects. As a result, the window of setting time (time
between initial and final setting) is narrower with the materials from US 63 bypass
(Ottumwa, IA).

The areas under the temperature-time curves within different time periods were also
analyzed and the results (with the columns referring to the value from original field mixes
and the error bars referring to the maximum and minimum values from mixes with
different levels of WR and FA) are shown in Figure 53. The figure illustrates that the area
under the calorimeter curves from three projects had similar trends in the first 24 hours.
However, in the Ottumwa (IA) Mix 1, area D (18 hours–24 hours) reduced when
compared with area C (12 hours–18 hours). This implies that the heat generation slowed
down after 18 hours.

200 1500

1250 Area X (1day)

150 Area Y (2day)
1000
Area, oFxh
Area, oFxh

100 750

Area A (1-6h) 500

50 Area B (6-12h)
Area C (12-18h) 250
Area D (18-24h)
0 0
US63 bypass US63 bypass

Figure 53. Areas under AdiaCal test curves of US 63 bypass (Ottumwa, IA) projects
during different test period

66
 14

Estimated, h

±0.781305
11.56217
12

IS-
10
8
18

Estimated, h
17

±0.653588
15.05554
16

FS-
15
14
13
5
±0.203096
3.51115
FS-IS, h

2
30
±0.634792
Temp, oC
27.44447

29
Peak

28
27
26
2
3
4
5
6

10
15
20
25
30
4
WR (fl 20.096
oz/cwt) SCMs/(c&SCMs)%

Figure 54. Statistical analysis from the US 63 bypass (Ottumwa, IA) AdiaCal robust
test

Statistical analyses were performed to study the effect of the amount of WR and FA
replacement on the initial and final thermal set time, the mortar setting window (FS-IS),
and peak temperature of AdiaCal tests. Least square fit was performed in the analysis of
these calorimeter test values. Different from US 71 and HW 95 projects, as shown in
Figure 54, the effects of FA replacements and WR on the initial and final thermal set time
in US 63 bypass mixes are significant. The figure also suggests that the setting window
reduced with the increased FA replacement levels; however, no significant changes on
the setting window were found with the changes in amount of WR. The peak temperature
from the AdiaCal test reduced with the FA replacement and WR dosage.

4.2.3.2 Isothermal Robust Test Results

Similar to US 71 (Atlantic, IA) and HW 95 (Alma Center, WI) mix, the isothermal tests
were performed for 72 hours at the testing temperature of 10oC, 48 hours at the testing
temperature of 20oC, and 24 hours at the testing temperature of 30oC and 40oC. Figure 55
shows that with the increase of the testing temperature, the maximum rate of heat
generation increases, while the time to reach this maximum rate decreases. The initial
thermal set times increased from 4.1 hours to 18.5 hours when the temperature dropped
from 40oC to 10oC. The final thermal set time increased from 5.8 hours to 25.7 hours
when the temperature dropped from 40oC to 10oC.

67
Figure 55. Isothermal test results for US 63 bypass (Ottumwa, IA) mix 1 at different
temperatures

Isothermal calorimeter test results from the robust tests are shown in Figure 56. The
detailed information on the thermal set time and the area under the heat generation curves
during different time periods for each mix can be found in
Table C.9.–34.

68
69
Figure 56. Isothermal robust test results of US 63 (Ottumwa, IA) mortar mixes at different temperatures

69
All calorimetry curves, from the mixtures with different WR dosages and FA
replacement levels, displayed a regular calorimetry curve shape and possessed a certain
peak height and width, which indicates that there is no incompatibility problem in the
concrete mixtures in the ranges of WR and FA applied. Results showed that the initial
thermal set time of Ottumwa (IA) mixes are between 18.5 hours and 22.4 hours at the test
temperature of 10oC, between 8.6 hours and 12.9 hours at the test temperature of 20oC,
between 6.9 hours and 8.2 hours at the test temperature of 30oC, and between 4.1 hours
and 6.9 hours at the test temperature of 40oC. The final thermal set times are between
25.7 hours and 31.4 hours at the test temperature of 10oC, between 13.2 hours and 18.5
hours at the test temperature of 20oC, between 9.7 hours and 11.2 hours at the test
temperature of 30oC, and between 5.8 hours and 8.2 hours at the test temperature of 40oC.

The boundaries of the initial and final thermal setting times from the isothermal robust
tests were summarized in Figure 57. Results showed that the initial and final thermal set
times and the setting time window all increase with the decrease of the environmental
temperature. Again, the variation of the thermal set time is generally increased with the
testing temperature. Similar to the US 71 (Atlantic, IA) and HW 95 (Alma Center, WI)
projects, the variation of the thermal set time values generally decreased with the
increased testing temperature. Also, unlike the AdiaCal test results, the variation of the
initial thermal set time was not clearly different from that of the final thermal set times.

40
US63 bypass (Ottumwa, IA)
Isothermal set time, hours

IS
30 FS
FS-IS

20

10

0
10oC 20oC 30oC 40oC
Testing temperature

Figure 57. Estimated set time from isothermal robust test on US 63 bypass
(Ottumwa, IA) mixes

The areas under the heat-generation time curves within different time periods were also
analyzed. Results in Figure 58 showed that the curves from three projects showed similar
trends in the first 24 hours. Generally, more heat was generated when the environmental
temperature was higher. At low temperature (10oC), the area increased with the time
elapse within the first 24 hours, which indicated more heat was generated. However, the
heat generation within 24 hours to 48 hours is higher than the first 24 hours after cement
made contact with water. The heat generation was found to be earlier and higher
compared to the other two projects. The heat generation slowed down after 12 hours at
30oC and 40oC.

70
 40 80 US63 bypass
Area A (1-6h) US63 bypass
(Ottumwa, IA)
Area B (6-12h) (Ottumwa, IA)
Area, mWxh/g 30 Area C (12-18h) 60

Area, mWxh/g
Area D (18-24h)

20 40
Area X (1day)
Area Y (2day)
10 20
Area Z (3day)

0 0
10oC 20oC 30oC 40oC 10oC 20oC 30oC 40oC
Testing temperature Testing temperature

Figure 58. Heat generation from isothermal robust test mixes at different times US
63 bypass (Ottumwa, IA) mixes

Least squares fit was performed on the prediction of thermal initial set (IS) and final set
(FS) time, setting time window (FS-IS) and peak heat generation from isothermal test
using the parameters of WR dosage, FA replacement percentage and environmental
temperature. According to the results as shown in Figure 59, similar to the finding from
the other two fields, the environmental temperature has the most significant effect on the
initial and final thermal set times and the peak heat generation rate. Both initial and final
thermal set times decrease when the environmental temperature goes up, setting time
window (from initial setting to final setting time) also reduces with the increase of
environmental temperature. The initial setting and final setting time both increase with
the amount of WR used and the percent replacement of the FA. The setting time window
can be reduced, increased or no obvious change with the increase of percentage
replacement of FA and WR, depending on the change on initial and final thermal set
times. FA replacement and WR dosage do not have obvious effects on peak heat
generation rate from the isothermal test.

71
 20

9.772478
±0.67344
15

IS, h
10
5

30
±0.913757
14.01939
FS, h

20
15

5
11
9
4.247469
±0.38056
FS-IS, h

7
5
3
1
9
±0.251141
Peak Rate
4.827061

7
5
3
1
2
3
4
5
6

10
15
20
25
30
5

15
25

35
45
4 25
WR (fl 20.096 Env.
oz/cwt) SCMs/(c&SCMs)% Temp. (oC)

Figure 59. Effect of mix design and temperature on IS and FS from isothermal
robust test (US63 bypass (Ottumwa, IA) mixes)

4.2.3.2 IQ Drum Test Results

The semi-adiabatic calorimetry test result is shown in Figure 56. The generated heat was
about 130 BTU/g cementitious materials at 150 hours, which was quite similar to the
result from the field test. This indicated a very good consistency of the IQ Drum test.

72
 Figure 60. IQ Drum test result of US 63 bypass (Ottumwa, IA) Mix 1

4.2.3.3 ASTM C403 Set Time Test Results

The relationships between thermal set times and ASTM C403 set times have been studied
previously. Here is another verification of the relationships. Only the materials collected
from Ottumwa (IA) were tested using the ASTM C403 method. The initial and final set
times of the nine mixes used for the isothermal robust tests were tested and the results are
shown in Table 13.

Table 13. ASTM set time result from robust test (US 63 (Ottumwa, IA) mixes)
Robust mix number 1 2 3 4 5 6 7 8 9
ASTM initial setting (hr) 7.8 9.3 6.5 8.3 6.7 9.3 8.3 8.4 5.8
ASTM final setting (hr) 10.1 11.7 8.8 10.9 8.9 14.6 11.0 10.6 8.2

The results show that the initial set time of the mixes is between 5.8 hours and 9.3 hours,
while the final set times are between 8.2 hours and 14.6 hours. Statistical analysis was
performed in order to study the effect of the amount of WR and FA replacement on the
ASTM initial and final setting. According to the results as shown in Figure 61, the initial
setting and final setting time increase with the amount of WR used and the percent
replacement of the FA. Also, the setting time window (from initial setting to final setting
time) increased with the increase of percentage replacement of FA and WR.

73
 10
9

±0.391138
7.822197
8

IS, h
7
6
5
16

±0.609725
14

10.53329
FS, h
12
10
8
6
±0.699393
5
2.711097
FS-IS, h

4
3
2
1
2
3
4
5
6
7
5
10
15
20
25
30
35
4
WR (fl 20.096
oz/cwt) SCMs/(c&SCMs)%

Figure 61. Effect of mix design on ASTM setting time US63 bypass (Ottumwa, IA)
mixes

4.3 Comparison of Lab Test Results from Different Projects

4.3.1 AdiaCal Tests

As mentioned previously, AdiaCal semi-adiabatic calorimetry tests were performed with

materials collected from all three projects at room temperature. The results from Mix 1
(the original field concrete mix proportion) tests of the three projects are summarized in
Figure 62. Similar to the results from field site tests, concrete samples made with
Ottumwa (IA) materials reach peak temperature earlier than samples made with Atlantic
(IA) and Alma Center (WI) materials. However, the differences in the peak temperatures
of these three mixes are not significant.

74
 Figure 62. AdiaCal calorimetry results from different projects (Mix 1)

4.3.2 Isothermal Tests

Isothermal robust calorimetry tests were performed with materials collected from all
three projects at four different temperatures. The rate of heat generation curves of
samples with three original mix designs are summarized in Figure 63. It is found that
similar shapes of heat generation curves were presented at all different temperatures.
Similar to the results from the field test, samples made with Ottumwa (IA) materials
reached peak heat of generation rate earlier than samples made with Atlantic (IA) and
Alma Center (WI) materials. Also, the peak rate of heat generation is slightly higher. The
results are consistent with the finding from AdiaCal tests.

75
76
Figure 63. Isothermal test results of mortar mix 1 of three projects at different temperatures

76
4.3.3 Set Time Results Comparison

Thermal set time from the AdiaCal thermometry test and isothermal thermometry at 20oC
was compared. As shown in Figure 64, thermal set time from both tests are generally in
agreement. Similar results were found from the thermal set time from the AdiaCal and
isothermal calorimetry tests. The thermal set times from nine Ottumwa mixes were also
compared with ASTM 403 set times. As shown in Figure 65, results from both tests are
generally in agreement with the ASTM test results. However, the relationship is not as
good as it was found to be from the field test. The relative big variation may be caused by
the difference of concrete and mortar mixing and the bigger variation of the WR dosage
and the FA replacement.

25 35

y = 0.8224x + 3.5385 30 y = 0.4507x + 10.721

20 2
R2 = 0.4859
AdiaCal initial set time, h

R = 0.6977

AdiaCal final set time, h

25
15
20

10 15

10
HW95 (Alma Center, WI) HW95 (Alma Center, WI)
5
US71 (Atlantic, IA) US71 (Atlantic, IA)
5
US63 Bypass (Ottumwa, IA) US63 Bypass (Ottumwa, IA)
0 0
0 5 10 15 20 25 0 5 10 15 20 25 30 35
Isothermal initial set time, h Isothermal final set time, h

Figure 64. Comparison of isothermal and AdiaCal set time results

20 20
Initial set Initial set
Final Set Final Set
16 Linear (Initial set) 16 Linear (Initial set)
y = 0.6521x + 1.0358
ASTM setting time, hour
ASTM setting time, hour

Linear (Final Set) Linear (Final Set) 2

y = 1.0616x - 5.456 R = 0.8236
2
R = 0.5364
12 12

8 8

4 y = 0.5279x + 1.7142 4 y = 0.417x + 3.7063

2 2
R = 0.7469 R = 0.6209

0 0
0 5 10 15 20 0 5 10 15 20
AdiaCal setting time, hour Isothermal setting time, hour

Figure 65. Comparison of ASTM and thermal set time results

77
5. HIPERPAV PREDICTION OF CONCRETE PERFORMANCE

In this section, a procedure for characterizing the hydration curve from both isothermal
and semi-adiabatic test data is presented. As a result of the procedure, heat of hydration
parameters for a mixture can be ascertained and used as inputs in the HIPERPAV
software to predict performance of concrete containing the same mixture.

5.1 Introduction

Under adverse environmental conditions, concrete pavements may be affected by large

temperature differentials and moisture loss resulting in premature cracking. HIPERPAV
is a software product developed for the Federal Highway Administration (FHWA) to
serve as a tool in the identification and control of the numerous factors affecting concrete
pavement behavior at early ages. HIPERPAV assesses concrete behavior within the first
72 hours based on materials used for the mix, design parameters, weather conditions, and
curing techniques. HIPERPAV directly considers the effects of: temperature development
in concrete, creep, relaxation, drying, thermal, and autogenous shrinkage. A detailed
description of HIPERPAV can be found elsewhere (5,6,7,8).

HIPERPAV predicts the temperature and moisture development in concrete pavements as

a function of hydration and climatic conditions. Temperature and moisture changes result
in stress development in the slab and are related to the development of strength. If
stresses are higher than strength, cracking is likely to occur.

The results from the HIPERPAV analysis can be used for concrete quality control,
optimization of pavement designs, prediction of pavement performance, and to help
contractors manage the temperature of concrete based on the concrete mixture designs
and specific climate and project conditions. The proposed study will facilitate
applications of both the HIPERPAV program as well as calorimeter tests in the concrete
pavement industry.

Currently, the HIPERPAV program predicts the concrete temperature development (heat
evolution) based on materials’ properties including cement characteristics (from a
database of the chemical compositions of cements and cementitious materials), type of
admixtures used, aggregate thermal properties, and concrete mixture proportions. In
HIPERPAV, concrete heat evolution is fundamental for the prediction of the pavement
concrete set time, strength, and stress development during the early age. In this project, a
method to characterize heat evolution from calorimetry test data was evaluated and the
HIPERPAV program was modified to use this information as an alternate method to
improve reliability of the HIPERPAV analysis. (That is, in this project, the HIPERPAV
program was modified to include the inputs for characterization of the heat evolution of
concrete mixtures. Thus, users will have the ability to directly enter heat evolution
parameters obtained from a calorimetry test for the concrete strength and stress analysis.)

To understand the evaluation of the method to characterize heat evolution and how it is
incorporated into HIPERPAV, it is important to first understand the basics of activation

78
energy.

5.2 Activation Energy

Activation energy ( Ea ) is the minimum amount of energy required for a material to

undergo a chemical reaction. A cement’s Ea is a critical material parameter in evaluating
its hydration characteristics. Therefore, it is computed in this section and will be utilized
in the hydration study presented later.

5.2.1 Method to Determine Activation Energy

Different methods for computing Ea include ASTM C1074 from strength testing—both
an incremental method and a linear approximation method (10)—and it can also be
derived from the Arrhenius equation. For the purpose of this research project, Ea was
computed based on the Arrhenius equation and isothermal test results as follows (11).

Step 1: Locate a maximum rate of heat evolution Pmax (W/g) for each test temperature
(T1, T2, T3, and T4) from the isothermal test results, as shown in Figure 66. It is regarded
that Pmax would happen at the same heat state Q (J/g) for different test temperatures of the
same material (12), and thus these peak points are utilized for computing Ea .

Rate of heat evolution P (W/g)

T1
T2
T3
T4

Heat Q (J/g)

Figure 66. Locate maximum hydration rate

Step 2: Determine a liner relationship between the natural-logarithmic-scaled Pmax and

the inverse of temperature (K). The Arrhenius equation, a formula accounting for the rate
of temperature-dependent chemical reaction (here it is referred to as the rate of heat
evolution), is defined as follows:

79
 Ea
−
P(T ) = Ae RT
(5-1)
where A = the pre-exponential factor
T = temperature (K)
R = gas constant (8.3144 J/mol/°C)

The natural-logarithmic scale is applied to both sides of equation 5-1:

⎛E ⎞ 1
Ln[P (T )] = Ln ( A) − ⎜⎜ a ⎟⎟ (5-2)
⎝ R ⎠T
Equation 5-2 shows that the Ln(P(T)) follows a linear function with 1/T.

Therefore, the activation energy can be determined from the slope of this linear function:
A
E a = RT ⋅ Log (5-3)
P
− Ea
The slope of the linear relationship can be achieved from the isothermal test results
R
of P versus T , as shown in Figure 67 (at least two temperature points are needed to
determine a slope).

Ln (P)

Slope

1/T (1/K)

Figure 67. Determine a linear relationship

5.2.2 Results of Activation Energy

The isothermal test results at four temperatures of cement mortar from three sites (Alma
Center, Atlantic, and Ottumwa) were utilized to compute Ea. The natural-logarithmic-
scaled P values versus 1/T values are presented in Figures 68–70. The values indicate a
linear function. Subsequently, Ea is calculated using the slope of those linear functions
based on the method described in section 5.1.1, and the results are reported in Table 14
and Figure 71.

80
These calculated Ea using this approach range from 41,581 J/mol to 52,664 J/mol, which
are close to those values reported by other researchers. Ea ranges from 30,000 J/mol to
62,000 J/mol based on the strength testing (13). Ea ranges from 33,500 J/mol to 41,000
J/mol (12).

The results show mixtures used at the Alma Center have the highest Ea , then Atlantic and
Ottumwa. The addition of a WR improves Ea (sample 2 compared to 1), and vice versa
(sample 3 compared to sample 1). Adding FA (reducing cement) slightly increases the
Ea (sample 4 compared to sample 1). Sample 9 has the lowest Ea (Sample 1–50% WR,
50%–FA).

Acitiviation energy computation

2.5
Alma Center -1
2.0 Alma Center -2
Alma Center -3
1.5 Alma Center -4
Alma Center -5
1.0 Alma Center -6
Ln (P)

Alma Center -7
0.5 Alma Center -8
Alma Center -9
0.0

-0.5

-1.0
0.00315 0.00320 0.00325 0.00330 0.00335 0.00340 0.00345 0.00350 0.00355 0.00360 0.00365

1/T

Figure 68. Activation energy calculation for AlmaCenter site (nine mixes, at four
temperatures: 5 oC, 20 oC, 30 oC, and 40oC; P unit: mW/g; T unit: K).

81
 Activiation energy computation
2.5
Atlantic - 1
Atlantic - 2
2.0 Atlantic - 3
Atlantic - 4
1.5
Atlantic - 5
Atlantic - 6
Ln (P)

Atlantic - 7
1.0 Atlantic - 8
Atlantic - 9
0.5

0.0
0.00315 0.00320 0.00325 0.00330 0.00335 0.00340 0.00345 0.00350 0.00355
1/T

Figure 69. Activation energy calculation for Atlantic site (nine mixes, at four
temperatures: 10 oC, 20 oC, 30 oC, and 40oC; P unit: mW/g; T unit: K).

Activiation energy computation

2.5
Ottumwa - 1
Ottumwa - 2
2.0 Ottumwa - 3
Ottumwa - 4
Ottumwa - 5
1.5
Ottumwa - 6
Ln (P)

Ottumwa - 7
1.0 Ottumwa - 8
Ottumwa - 9

0.5

0.0
0.00315 0.00320 0.00325 0.00330 0.00335 0.00340 0.00345 0.00350 0.00355

1/T

Figure 70. Activation energy calculation for Ottumwa site (nine mixes, at four
temperatures: 10 oC, 20 oC, 30 oC, and 40oC; P unit: mW/g; T unit: K)

82
Table 14. Calculated activation energy (Unit: J/mol).

Sample 1 2 3 4 5 6 7 8 9
site
Ottumwa 43227 42160 41805 42414 43250 42212 45072 42021 41581
AlmaCenter 47386 52664 47285 52930 48640 52599 48015 49288 42429
Atlantic 43344 44378 42587 48643 42643 48467 42842 47527 42794

Activiation energy
60000
Ottumwa
AlmaCenter
50000
Activiation energy (J/mol)

Atlantic

40000

30000

20000

10000

0
1 2 3 4 5 6 7 8 9
Sample No.

Figure 71. Calculated activation energies for nine mixes at three sites based on the
isothermal test results

5.3 Hydration Curve Parameters Based on Isothermal Test

The rate of heat evolved during cement hydration is called degree of hydration (DOH).
The hydration curve parameters are used to characterize DOH and compute the heat
evolution of cementitious materials. In this section, the hydration curve parameters of
cement mortar are computed based on the isothermal test results, as detailed in the
following.

5.3.1 Computation Approach

The degree of hydration can be determined according to the generated heat and total heat
at a specific point in time (12):

83
 Q(t )
α (t ) = (5-4)
Hu
where Q(t) is the accumulated heat evolved at the time t during the hydration procedure
and Hu is the total heat of the specific cementitious material.

H (u ) is determined using the following equation (7):

H (u ) = H cem ⋅ p cem +461 ⋅ p slag +1800 ⋅ p FA−Cao ⋅ p FA (5-5)

The time t is usually converted to an equivalent age that expresses the maturity of
cementitious material during the hardening procedure. The well-known equivalent age
formula (9) is adopted in this research:
Ea 1 1
− ⋅( − )
Δt e (Tr ) = e
R Tc Tr
⋅ Δt (5-6)

Where, Tc = the temperature (K),

Tr = the reference temperature,
Ea = activation energy that is computed in section 5.2.

The following equation to characterize cement hydration is utilized (9):

⎛ ⎡τ ⎤β ⎞
α (t e ) = α u ⋅ exp⎜ − ⎢ ⎥ ⎟ (5-7)
⎜ ⎣ te ⎦ ⎟
⎝ ⎠

Where, α(te) = degree of hydration at equivalent age, te,

te = equivalent age at reference temperature (21.1°C), (hrs),
αu = ultimate degree of hydration,
τ = hydration time parameter (hrs), and
β = hydration shape parameter.

A larger αu indicates a higher DOH (Figure 72), and a larger τ implies a larger delay of
hydration (Figure 73). The slope of the major linear part of the hydration shape is
represented by β; a larger β implies a higher hydration rate (Figure 74).

84
Figure 72. Influence of hydration curve parameter αu on degree of hydration

Figure 73. Influence of hydration curve parameter β on degree of hydration

85
 Figure 74. Influence of hydration curve parameter τ on degree of hydration

The natural-logarithmic scale is applied to Equation 5-7:

β
⎡τ ⎤
Ln[α (t e ) ]= Ln(α u ) − ⎢ ⎥ (5-8)
⎣ te ⎦

Log {Ln (α u ) − Ln[α (t e ) ]} = β log τ − β log t e (5-9)

Equations 5–9 show log{log (α u ) − log[α (te ) ] } has a linear relationship to log te , thus, the
parameter of β can be determined from the slope; and τ can be achieved from the
intersection point of this linear function.

The degree of hydration is computed using Equation 5-4 at different equivalent ages, and
then compared with the theoretical results using equation 5-5. Curve fitting and back-
calculation are performed to achieve these hydration curve parameters, which are realized
using the optimization method through the Solver function embedded in Microsoft Excel
2003. The computation procedure with the sample-5 at the Alma Center is detailed in the
following paragraph.

First, the rates of heat evolution results from isothermal test data are pre-processed. There
exists a peak area at the initial stage due to temperature equilibrium at the test set-up as
shown in Figure 75. This peak area is relatively small and difficult to be accurately
accounted for; thus, it is removed for the heat computation. A straight line is used to
connect the start points and the valley points after those peak areas (Figure 75).

86
 Peak area

Figure 75. Pre-process the data of rate of heat evolution from isothermal tests

Subsequently, the generated heat from time ti to time ti+1 is calculated using the
trapezoidal method as shown in Figure 76. The heat Q(t) is calculated as follows:

ΔQ(t ) =
[P(t i ) + P(t i )]× (t i
+1 +1 − ti )
=
[P(t i ) + P(t i )]× Δt
+1
(5-10)
2 2

Therefore, the accumulated heat at each time point can be calculated as follows:

Q(t i +1 ) = Q(t i ) + ΔQ (5-11)

Equation 5-9 is substituted into Equation 5-4 to determine the DOH. (Note: These
DOH values will be called as “measured values” in order to compare with the
predicted ones from Equation 5-7).

87
 Pi +1

Pi
ΔQ(t )

t i t i +1

Figure 76. Heat computation based on the trapezoidal method

The determined DOH, α, is compared with the theoretical calculated results using a group
of seed values of hydration curve parameters based on Equation 5-7, and the curve fitting
and optimization method are utilized to achieve the hydration curve parameters (αu, τ, and
β). As an example, the curve fitting results at four temperatures of sample-5 at Alma
Center are presented in Figures 77–80. The calculation is performed at each temperature
for each mix at each site.

88
Figure 77. Predicted degree of hydration vs. measurements at 5 oC (Sample 5, Alma
Center)

Figure 78. Theoretical degree of hydration vs. measurements at 20 oC (Sample 5,

Alma Center)

89
 Figure 79. Predicted degree of hydration vs. measurements at 30 oC (Sample 5,
Alma Center)

Figure 80. Predicted degree of hydration vs. measurements at 40 oC for (Sample 5,

Alma Center)

5.3.2 Calculation Results

The back-calculated hydration curve parameters for all mixes at three sites are presented
in Tables 15–17. The mean values of hydration curve parameters at 20 oC, 30 oC, and
40oC (Alma Center and Atlantic), and 30 oC and 40oC (Ottumwa) are also presented since

90
they will be utilized in the pavement temperature computation as discussed later. The
back-calculation is performed considering three temperatures (20 oC, 30 oC, and 40oC) at
the same step. It should be noted that at 5 oC, the back-calculated αu is sometimes larger
than one; thus it is controlled to be less than one during the optimization procedure. The
results of the back calculation show adding WR would increase the hydration rate while
increasing FA content reduces the hydration rate, and τ increases with increasing
temperature.

Table 15. Hydration curve parameters calculated based on isothermal test results
(Alma Center, WI)
20 oC– Average 20 oC,30
o o o o
Sample no. Parameters 5C 20 C 30 C 40 C 40oC[1] o
C,40oC
αu 0.9900 0.6108 0.6252 0.5959 0.5586 0.6106
1 β 0.7035 1.6408 1.7508 1.9374 1.8504 1.7763
τ 29.3885 20.2465 25.9669 29.4758 22.8392 25.2297
αu 0.7162 0.6212 0.6618 0.6592 0.7155 0.6474
2 β 1.9342 1.7294 1.8644 1.9366 1.9342 1.8435
τ 20.1814 20.0513 29.1004 36.7210 20.1814 28.6242
αu 0.9579 0.5905 0.6044 0.5761 0.4749 0.5903
3 β 0.7035 1.6408 1.7508 1.9374 2.1456 1.7763
τ 29.3885 20.2465 25.9669 29.4758 31.8346 25.2297
αu 0.9900 0.5935 0.7216 0.6600 0.6216 0.6785
4 β 0.6940 1.7758 1.6676 1.6379 1.6936 1.6937
τ 31.3042 21.7487 30.3611 34.4732 28.8627 28.8611
αu 0.9900 0.6992 0.7216 0.6051 0.5717 0.6753
5 β 0.6881 1.3610 1.4878 1.8616 1.8107 1.5701
τ 28.8024 19.7491 24.5006 26.9429 20.0933 23.7309
αu 0.9900 0.4688 0.4988 0.6068 0.4129 0.5248
6 β 0.7971 2.0843 1.7205 1.4647 1.9857 1.7565
τ 36.6549 22.6095 29.2576 45.8113 24.9138 32.5595
αu 0.9900 0.6476 0.6638 0.6097 0.5810 0.6404
7 β 0.7503 1.5567 1.6415 2.0698 1.8125 1.7560
τ 30.0142 20.0987 23.7024 29.1781 21.4137 24.3264
αu 0.6751 0.5376 0.6052 0.6196 0.5416 0.5875
8 β 0.8907 1.8083 1.7062 1.7566 1.7717 1.7570
τ 19.8322 20.3703 24.8406 32.6339 22.9035 25.9483
αu 0.5684 0.7181 0.6961 0.6093 0.6101 0.6745
9 β 1.0399 1.2447 1.3566 1.7380 1.5778 1.4464
τ 16.2371 18.9216 20.2745 21.6115 18.2808 20.2692

Note: [1] back-calculation considering three temperatures at the same step

91
Table 16. Hydration curve parameters back-calculated based on isothermal test
results (Atlantic, IA)
20 oC– Average 20 oC,30
o o o o
Sample no. Parameters 5C 20 C 30 C 40 C 40oC C,40oC
o

αu 0.9900 0.6060 0.5801 0.5371 0.5066 0.5744

1 β 0.9277 1.6992 1.9421 2.2421 2.1927 1.9611
τ 26.6044 18.3391 20.8226 27.2633 19.2624 22.1417
αu 0.9140 0.5866 0.5433 0.5154 0.4882 0.5484
2 β 1.0957 1.7944 2.2946 2.4197 2.4049 2.1696
τ 24.5420 19.1539 22.5632 27.8291 20.7546 23.1821
αu 0.7909 0.6224 0.6010 0.5324 0.5152 0.5853
3 β 1.1247 1.6220 1.7726 2.0871 2.1575 1.8272
τ 20.2132 18.0107 18.9814 22.5658 17.7784 19.8526
αu 0.8611 0.5415 0.5187 0.5402 0.4880 0.5335
4 β 1.1201 2.2463 2.4873 2.3114 2.5121 2.3483
τ 21.0165 20.5071 22.9329 30.2924 22.0432 24.5775
αu 0.7828 0.6538 0.6811 0.6034 0.5080 0.6461
5 β 1.0529 1.4173 1.7726 2.0871 2.0441 1.7590
τ 14.6331 19.1543 20.4121 26.2018 18.1415 21.9227
αu 0.9308 0.5255 0.5085 0.5287 0.4604 0.5209
6 β 1.1511 2.3990 2.6702 2.3426 2.7631 2.4706
τ 25.1907 22.1607 25.1194 32.8242 23.6658 26.7014
αu 0.7630 0.6304 0.5698 0.5097 0.4991 0.5700
7 β 1.1755 1.6402 1.9223 2.3287 2.2734 1.9637
τ 21.9671 19.5463 21.3133 24.7369 19.6538 21.8655
αu 0.7248 0.5791 0.5573 0.5433 0.5032 0.5599
8 β 1.2721 1.8846 2.1994 2.2006 2.3164 2.0949
τ 17.8805 18.1573 21.1945 27.0361 19.8111 22.1293
αu 0.7868 0.7255 0.6719 0.5575 0.5617 0.6516
9 β 1.0066 1.1372 1.3372 1.7853 1.6398 1.4199
τ 20.0718 17.8486 19.6514 20.5597 16.7853 19.3532

92
Table 17. Hydration curve parameters back-calculated based on isothermal test
results (Ottumwa, IA)
20 oC–
o o o o
Sample no. Parameters 5C 20 C 30 C 40 C 40oC Average 30 oC,40oC
αu 0.5598 0.5295 0.4905 0.6312 0.5798 0.6312
1 β 1.4649 1.6057 1.9539 1.4170 1.4467 1.4170
τ 9.3784 14.2056 16.6248 20.4194 17.6295 20.4194
αu 0.5878 0.5012 0.4618 0.6254 0.5470 0.6254
2 β 1.5765 1.9010 2.3930 1.5472 1.7191 1.5472
τ 12.1947 16.0293 18.3387 25.2515 19.4279 25.2515
αu 0.5637 0.5517 0.5342 0.6072 0.5898 0.6072
3 β 1.4340 1.4857 1.6847 1.8907 1.3580 1.8907
τ 9.1983 12.9745 14.3461 25.0715 16.0093 25.0715
αu 0.5381 0.4997 0.4615 0.6152 0.5587 0.6152
4 β 1.4980 1.6355 2.0229 1.5335 1.4637 1.5335
τ 10.6448 15.4495 16.8088 25.1642 18.9353 25.1642
αu 0.6140 0.5061 0.5177 0.6390 0.5882 0.6390
5 β 1.3743 1.7233 1.9534 1.4710 1.4826 1.4710
τ 9.5829 14.3867 15.0166 20.4169 16.7574 20.4169
αu 0.5618 0.4712 0.4525 0.5916 0.5882 0.5916
6 β 1.4423 1.8693 2.1951 1.7298 1.4826 1.7298
τ 12.0907 17.4293 18.3742 29.3694 16.7576 29.3694
αu 0.6316 0.5354 0.4866 0.6348 0.5680 0.6348
7 β 1.3625 1.9418 2.3196 1.7158 1.7611 1.7158
τ 11.6373 15.6103 17.1054 24.8943 18.4770 24.8943
αu 0.5404 0.5193 0.5039 0.6174 0.5425 0.6174
8 β 1.4114 1.5082 1.7221 1.3677 1.4599 1.3677
τ 9.4450 14.0397 14.7238 22.4863 15.9444 22.4863
αu 0.6319 0.6032 0.5634 0.6469 0.5856 0.6469
9 β 1.2789 1.3351 1.5969 1.3721 1.4361 1.3721
τ 8.9879 11.6651 13.2458 19.8030 13.5333 19.8030

It is also noted that the total heat Hu would affect the hydration curve parameters,
requiring that sensitivity analysis be performed. Hu ranges from 370 J/g to 513 J/g based
on the 21 mixes (15). In this study, Hu ranging from 250 to 467 J/g is utilized for the
sensitivity analysis. These results shown in Table 18 indicate that αu increases, while β
and τ decrease as Hu decreases.

93
Table 18. Sensitivity of hydration curve parameters to total heat

(1) Hu: 467 J/g

20 oC–40 Average 20 oC,30
o o o o o o
5C 20 C 30 C 40 C C C,40oC
αu 0.9900 0.6108 0.6252 0.5959 0.5586 0.6107
β 0.7035 1.6408 1.7508 1.9374 1.8504 1.7764
τ 29.3885 20.2465 25.9669 29.4758 22.8392 25.2297

(2) Hu: 414 J/g

20 oC–40 Average 20 oC,30
o
5oC 20oC 30oC 40oC oC C,40oC
αu 0.9900 0.6886 0.7048 0.6718 0.6298 0.6884
β 0.7559 1.6408 1.7508 1.9374 1.8504 1.7763
τ 25.2348 20.2466 25.9669 29.4760 22.8392 25.2298

(3) Hu: 250 J/g

20 oC–40 Average 20 oC,30
o o
5oC 20oC 30oC 40oC C C,40oC
αu 0.9900 0.9900 0.9900 0.9900 0.9900 0.9900
β 1.1033 2.0642 2.1479 2.4760 2.0287 2.2294
τ 14.4082 18.5720 23.5986 27.7870 22.1826 23.3192

5.4 Hydration curve parameters based on the semi-adiabatic test and HIPERPAV II
model

In this section the hydration curve parameters are back-calculated using the Semi-
adiabatic test results. The rate of heat evolution is calculated as follows (6,7,8):
⎛E ⎞⎞
β
⎡τ ⎤ ⎡β ⎤ ⎛ 1 1
⋅ exp⎜⎜ a ⎟⎟ ⎟ (5-12)
⋅⎢ ⎥ ⋅α ( te )
P (t e ) = H u ⋅ C p
⎢ ⎥
⎣ te ⎦ ⎣ te ⎦ ⎜⎜ − ⎟
⎝ R ⎝ 273.15 + Tr 273.15 + Tc ⎠⎠

where, P(te) = rate of heat liberation at equivalent age, te, (W/m3),

Hu = Total heat of hydration (J/kg)
Cp = the specific heat of cemetious material.
E = activation energy (J/mol),
R = universal gas constant (8.3144 J/mol/°C),

The theoretical hydration curve is calculated from using seed values of the hydration time
and shape parameters with the theoretical maximum temperature increase from the
hydration reaction estimated for that test. The time and shape parameters are then back-
calculated by minimizing the log of errors (differences) at every time step from the actual
hydration curve to the theoretical hydration curve. Afterwards, the effects of heat on the
developed stress and strain of pavement and material strengths are accounted for
(HIPERPAV II).

For concrete samples, the total heat of hydration is calculated by relating the mass and

94
specific heat of the concrete with the total temperature increase observed. The formula
for the total heat of hydration is given below in Equation 5-13.
mconcrete
Hu = • C p • ΔT (5-13)
mcement
Where,
mconcrete = mass of concrete (kg)
mcement = mass of cementitious material (kg)
Cp = specific heat of concrete (J/g⋅°C)
ΔT = total change in temperature (°C)

Subsequently, the temperature rise at the adiabatic condition can be determined as

follows:
P(t ) × (t i +1 − t i )
ΔT = (5-14)
Cc
Thus, the temperature at any point in time is determined as follows:
P(t ) × (t i +1 − t i )
Ti +1 = Ti + ΔT = Ti + (5-15)
Cc
The theoretical computed temperature is compared with the measured adiabatic
temperature at all time points, and curve fitting is performed through the optimization
method using the Solver function embedded in Microsoft Excel 2003 to achieve the
hydration curve parameters. The calculated temperatures versus measurements of four
concrete mixtures are presented in Figure 81. The calculated results of hydration curve
parameters are presented in Table 19.

95
 80

60
temperature (°C)
Adiabatic PCC

40

Measured

Calculated
20

0
0 24 48 72 96 120 144 168

Test Duration (hr)

Figure 81. Alma Center field concrete

96
 80

60
Temperature (°C)
Adiabatic PCC

40
Measured

Calculated
20

0
0 24 48 72 96 120 144 168

Test Duration (hr)

Figure 82. Alma Center lab concrete

97
 80

60
Temperature (°C)
Adiabatic PCC

40
Measured

Calculated
20

0
0 24 48 72 96 120 144 168

Test Duration (hr)

Figure 83. Atlantic Field concrete

98
 80

60
Temperature (°C)
Adiabatic PCC

40
Measured

Calculated
20

0
0 24 48 72 96 120 144 168

Test Duration (hr)

Figure 84. Ottumwa Field Concrete

Table 19. Back-calculated hydration curve parameters based on Semi-adiabatic test

Alma Center Alma Center Atlantic Ottumwa

field concrete lab concrete field concrete field concrete
αu 0.633 0.646 0.655 0.805
β 0.705 0.699 0.604 0.556
τ 33.292 33.022 32.502 35.380

Results seem to indicate the following: the calculated hydration curve parameter β, based
on the isothermal test data, is larger than that calculated using semi-adiabatic test data. β
values based on the semi-adiabatic tests are closer to the values reported by other
researchers (Schindler 2002) using the chemical-based empirical equation; and the
hydration curve parameter τ based on the isothermal test data seems to be smaller than
that of the semi-adiabatic test data. In order to evaluate these two groups of hydration
curve parameters, the HIPERPAV II software was used to predict the in situ pavement
temperatures.

5.5 Conversion from Isothermal to Semi-Adiabatic Calorimetry

Based on the limited tests, it would be meaningful to convert between the isothermal and
semi-adiabatic or full-adiabatic tests. However, there are very few studies presented on
this topic based on the authors’ literature review. Wadsö (12) developed a statistical

99
model, and Hatzitheodorou et al. (16) developed a model and computation procedure
based on the maturity to convert from the isothermal test to semi-adiabatic and full-
adiabatic for cement and cement mortar, respectively. In this research a mathematical
model and computation approach to convert the isothermal calorimetry of cement mortar
to semi-adiabatic calorimetry of cement concrete are developed, which has extended from
the basic methodology (12). The Visual Basic Application (VBA) program is utilized to
realize the computational procedure using finite difference method on the Microsoft
Excel 2003 platform. The model and computation procedure are detailed as follows with
an example of Alma Center:

Step 1: Pre-process the data of isothermal tests. The peak area at the initial early stage
due to temperature equilibrium is removed as discussed previously (Figure 75). At least
two tests at two temperatures are needed for this computation (e.g., in this project four
temperatures are used).

Step 2: Calculate the generated heat at each point in time. The trapezoidal method is used
to approximate the accumulated heat as shown in Equation 5-9 and Figure 76.

Step 3: P versus Q. The measured P(t) (W/g) vs. Q (J/g) are plotted as shown in Figure
85. Thus, at each Q point, the P points at different temperatures can be achieved. Since
the tests at different temperatures have different Q points, linear interpolation is utilized
to achieve the P points at any Q point. This method has good accuracy because the time
interval of recorded test data is very small (e.g., 0.01 hour).

(Pi +1 − Pi )
P (t ) = Pi + (t − t i ) × (5-16)
(t i +1 − t i )

100
 Isothermal P vs Q
9

7
5 oC
6 20 oC
Measured P (mW/g)

30 oC
40 oC
5

3
Unknown

0
1 21 41 61 81 101 121 141 161 181 201 221 241 261 281
Calculated Q (J/g)

Figure 85. P vs. Q

However, the test results might not provide a complete list of P vs. Q since the test may
stop before it reaches the maximum heat state Hu, as shown in Figure 85. Therefore, a
statistical regression is utilized to predict the trend of P vs. Q points at a longer time
period during hydration, and it shows that the exponential function could predict this
trend well. For example, the exponential function is used to predict the P vs. Q points for
those unknown areas at longer hydration time beyond the test range as illustrated in
Figure 86.

101
 Isothermal P vs Q
3.5

5 oC
3.0 20 oC
30 oC
40 oC
2.5 Expon. (5 oC) -0.0104x
Expon. (20 oC) y = 16.498e
Measured P (mW/g)

Expon. (30 oC) 2

R = 0.9992
Expon. (40 oC)
2.0
-0.0118x
y = 11.444e
1.5 2
R =
`
0.9133

-0.0191x
1.0 y = 29.093e
2
R = 0.956
-0.0115x
0.5 y = 2.0052e
2
R = 0.9866
0.0
0 20 40 60 80 100 120 140 160 180 200 220 240 260 280 300

Calculated Q (J/g)

Figure 86. Exponential equations to approximate P vs. Q

Step 4: P vs. T. A key concept to understanding this research is that at the specific heat
state (Q) and temperature state (T) for the cementitious material, the rate of heat
evolution (P) (hydration rate) is always the same, no matter if it is exposed to isothermal,
adiabatic or other testing regimes and environmental conditions. Therefore, the purpose
of this step is to achieve P vs. T at different Q states. The measured and linearly
interpolated P point at each Q point of four temperatures (Figure 87) is extracted to
approximate a relationship between P and T, and a multi-linear model is used to
approximate this relationship, as shown in Figure 88.

102
 P

T1

T2

T3
T4

Q
Qi

Figure 87. Extract P points at any Q state

P(Qi)

T4
⎧a1 + b1T , T ≤ T2
⎪
T3 PQ (T) = ⎨a 2 + b2T , T2 < T ≤ T3
⎪a + b T , T ≥ T
⎩ 3 3 3

T1 T2

Figure 88. Approximate P vs. T at any heat (Q) state

Step 5: Temperature is lost during the semi-adiabatic test. As shown in Figure 89, the
generated heat by cement hydration releases through the calorimeter wall into the
immediate environment. The temperature at the surface of the inside wall (Tin) is higher
than that at the surface of the outside wall Tout. According to Fourier's law, the rate of
heat conduction within a solid is determined as follows:
ΔQ T − Tout
P= = k × A × in (5-17)
Δt Δx
Where, k = thermal conductivity of calorimeter
A = surface area of calorimeter
Δx = the thickness of calorimeter wall.
Tin = temperature at the surface of inside wall
Tout = temperature at the surface of outside wall

103
Therefore, the heat loss of concrete through the release of calorimeter to the surrounding
environment at a time step can be calculated as follows:

Tin − Tout k×A

ΔQ = k × A × × Δt = × (Tin − Tout ) × Δt (5-18)
Δx Δx

Tin − Tout
ΔQCond = k × A × × Δt (5-19)
Δx
Accordingly, the temperature loss through calorimeter conduction at a time step is
computed as follows:

ΔQ ⎡ k × A ⎤
ΔTcond = =⎢ ⎥ × (Tin − Tout ) × Δt (5-20)
C p ⎢⎣ C p × Δx ⎥⎦

where, Cp = the heat capacity of concrete (J/kg·oC).

Calorimeter wall
Cement
Tin

Tout
Heat release

Figure 89. Heat conduction in the calorimeter wall

Heat convection happens between the outside surface of calorimeter and the surrounding
air. However, in order to simplify this computation procedure, it is assumed that the Tout
is the same as the temperature of air, and Tin is the same as that of the cement. In this
project, the semi-adiabatic tests were performed and the heat (temperature) losses are
k×A
estimated, thus the C = in Equation 5-20 as a material parameter (W/oC) can
C Con × Δx
be back-calculated.

Step 6: Determine temperature “absorbed” or “released” by the calorimeter. During the

temperature rise procedure, the calorimeter “absorbs” a portion of heat and during the
procedure of temperature decrease, it “releases” a portion of heat that is generated by
cement hydration. This part of heat also contributes to the semi-adiabatic temperature

104
decrease or rise.

The absorbed or released heat by the calorimeter can be calculated as:

ΔT
ΔQcalo = C calo × × M Calo (5-21)
2

where, Ccalo = the heat capacity of calorimeter (J/kg·oC)

MCalo = the mass of calorimeter (kg)
ΔT = the raised or decreased temperature (oC)

Therefore, the temperature loss or gain of concrete due to calorimeter absorption or

release can be determined as follows:

QCalo ⎡ C M ⎤
ΔTCalo = = ⎢0.5 × calo × Calo ⎥ × ΔT (5-22)
C p × M Con ⎢⎣ Cp M Con ⎦⎥

Where, Cp = the heat capacity of concrete (J/kg·oC)

MCon = the mass of concrete (kg)

C calo M Calo
Let R = 0.5 × × as a ratio parameter.
C con M Con

Therefore, the total temperature loss due to heat conduction through calorimeter to the
surrounding air and heat absorption or release of calorimeter can be calculated in the
following equation:

ΔQ ⎡ k × A ⎤ ⎡ C calo M Calo ⎤
ΔTLoss = =⎢ ⎥ × (Tin − Tout ) × Δt + ⎢0.5 × × ⎥ × ΔT (5-23)
C con ⎣ C con × Δx ⎦ ⎣ C con M Con ⎦

The modeled results of temperature loss using Equation 5-23 versus measurements are
shown in Figure 90.

105
 1.0

Estimated from measurements

0.8 Modeled

0.6
Temperature loss ( C)
o

0.4

0.2

0.0

-0.2

-0.4
0 20 40 60 80 100 120 140 160 180
Time (hr)

Figure 90. Calculated temperature losses versus measurement estimations

Step 7: Determine the semi-adiabatic temperature. Due to the heat balance at each heat
state (time point or temperature state), the total heat generated by the cement hydration
includes the one raising the temperature of concrete, the one released to the surrounding
environment through calorimeter conduction, and the one absorbed (during temperature
rise) or released (during temperature decrease) by the calorimeter. The heat balance at the
semi-adiabatic test is expressed as:

ΔQtot = ΔQT + ΔQCond + ΔQCalo (5-24)

Where Qtot is the total heat, QT is the heat in the cement which raises the temperature of
the concrete sample in the semi-adiabatic condition. The temperature rise of concrete at a
specific step is determined as:

ΔQtot
ΔT = − TLoss (5-25)
CCon

It should be noted that the isothermal test data are based on the cement mortar, while the
semi-adiabatic tests are based on cement concrete. Thus, generated heat evolution Q (J/g)
of cement mortar is converted to that of cement concrete. In this research an assumption
is proposed that during the hydration procedure, the temperatures are uniform for all
material components including cement paste, aggregates, and sands. Therefore, the
potential delay of temperature rise or decrease due to different heat conductivity of

106
material components is ignored. Based on this assumption, the heat evolution procedure
is the same for cement mortar (cement paste plus sand) and cement concrete (cement
paste, sand and aggregate) except that they have different mass, as illustrated in Figure
91. Therefore, the heat Q (J/g) of concrete can be determined in terms of the test results
of cement mortar:

M cem
Qcon = Qcem × (5-26)
M con

where Qcon = heat of concrete (J/g)

Qcem = heat of cement (J/g)
Mcon = mass of concrete (g)
Mcem = mass of cement (g)

Heat generation

Additives
Aggregate
Cement
Sand
Heat generation

Heat generation

Heat generation

Figure 91. Heat generation of cementitious material

The finite difference (FD) method is used to solve this computer procedure based on a
VBA program built on the Microsoft Excel platform. A heat step (ΔT) or time step (Δt)
can be used to run this procedure. When using a heat step, the time can be back-
calculated from Equation 5-8 as follows:

2Q(t )
Δt = (5-27)
P(t i ) + P (t i +1 )

When using a time step, a small time step such as of 0.01 hour is needed to assure the
accuracy of computation. The accumulated temperature at the jth time step is denoted

107
by T j , then the temperature at the next step is determined as follows:
T j +1 = T j + ΔT (5-28)

As an example, the forward FD method with regards to time steps (0.01 hour per step) is
used to simulate the temperature vs. time at the semi-adiabatic test from the isothermal
test results, as shown in Figure 92.

Figure 92. Simulated semi-adiabatic temperature (from isothermal data) vs.

measurements

The results show that the simulation from isothermal data has a reasonable agreement
with the measurements though there is some small delay at the early age.

The full-adiabatic temperature can also be simulated using this approach if the isothermal
test data includes the higher temperature levels necessary to approximate the temperature
of a full-adiabatic test condition. Without this high-level temperature, the rate of heat
evolution at the high-level temperature range is unknown, and the prediction of trend in
that range may induce significant errors.

However, after converting the isothermal calorimetry to the semi-adiabatic calorimetry,

the semi-adiabatic calorimetry data can be converted to the full-adiabatic calorimetry data
using the method (17).

108
The predicted semi-adiabatic temperatures can be used to back-calculate the hydration curve
parameters based on the method described in section 5.3. Subsequently, the pavement
temperature, stresses, and strength of concrete materials can be predicted using the HIPERPAV
software.

The computational procedure discussed by the previous paragraphs is summarized in Figure 93.

Isothermal tests

Heat loss to Heat generated by Heat absorption

environment cement hydration by calorimeter

Measurements at
several temperatures

Temperature in semi-
adiabatic condition
HIPERPAV II
models
Activation energy Temperature in
adiabatic condition
HIPERPAV II models
HIPERPAV Software Hydration
parameters

Pavement temperature Material strength Stress and strain

Figure 93. Flow chart of computation procedure

5.6 Modification of HIPERPAV Software

The HIPERPAV software was modified to allow users to define the inputs of hydration curve
parameters (αu, β, and τ). Originally, HIPERPAV computed hydration curve parameters based
on linear regression models as a function of cement chemistry (6,7,8). In this modified version,

109
users input values for the hydration curve parameters, as shown in Figure 94. HIPERPAV then
predicts hydration and pavement temperatures as a result of these inputs.

Figure 94. Windows of inputs of hydration curve parameters in the modified HIPERPAV
II software.

110
5.7 Prediction of Pavement Temperatures

The temperatures of in situ pavement at three sites (Alma Center, WI; Atlantic, IA; and
Ottumwa, IA) are predicted using the HIPERPAV II software. Increased temperatures due to
hydration are very important in calculating developed stresses and material strength in concrete
at early ages. The hydration parameters back-calculated from both the isothermal tests and semi-
adiabatic tests are used as inputs in HIPERPAV II software, in order to find which one would be
more reliable for predicting the pavement temperatures. The analysis and results are presented in
the following sections.

5.7.1 Alma Center Pavement Temperature and Prediction

5.7.1.1 Inputs

The weather information for temperature, wind speed, and humidity at the Alma Center in Iowa
were downloaded from the Weather Underground website (http://www.wunderground.com/) and
are shown in Figure 95–97.

Temperature-Alma Center, IA
100
90

80
70
Temperature ( C)

60
o

50
40
30
20
10
0
7/18/2007 4:48 7/18/2007 9:36 7/18/2007 14:24 7/18/2007 19:12 7/19/2007 0:00 7/19/2007 4:48

Date

Figure 95. Temperature at the Alma Center, IA

111
 Wind speed-Alma Center, IA
14.0

12.0

10.0
Wind speed (mile/hr)

8.0

6.0

4.0

2.0

0.0
7/18/2007 4:48 7/18/2007 9:36 7/18/2007 14:24 7/18/2007 19:12 7/19/2007 0:00 7/19/2007 4:48

Date

Figure 96. Wind speed at the Alma Center, IA

Humidity-Alma Center, IA
90

80

70

60
Humidity (%)

50

40

30

20

10

0
7/18/2007 4:48 7/18/2007 9:36 7/18/2007 14:24 7/18/2007 19:12 7/19/2007 0:00 7/19/2007 4:48

Date

Figure 97. Humidity at the Alma Center, IA

112
5.7.1.2 Results and Analysis

The predicted temperatures using both the hydration curve parameters back-calculated from
isothermal tests and semi-adiabatic tests are presented in Figure 98–100. The figures show
hydration curve parameters generated from semi-adiabatic test data better match actual pavement
temperatures than the curves generated by the isothermal test data. The temperatures using the
hydration curve parameters of isothermal tests have a delay at the first cycle due to a larger τ
value. Therefore, results using the semi-adiabatic test data are recommended by this research. It
should be noted that the measured pavement temperatures may have errors due to equipment and
environmental conditions.

Pavement temperature-Alma Center, WI

45

40

35

30
Temperatures ( C)
o

25

20

15 Measured Top

10 Isothermal Predicted Top

Adiabatic Predicted Top

5

0
7/18/2007 0:00 7/18/2007 12:00 7/19/2007 0:00 7/19/2007 12:00 7/20/2007 0:00 7/20/2007 12:00 7/21/2007 0:00 7/21/2007 12:00
Date

Figure 98. Predicted pavement temperatures versus measurements (pavement top, Alma
Center, WI )

113
 Pavement temperature-Alma Center, WI
45

40

35

30
Temperature ( oC)

25

20

15
Measured Mid
10
Isothermal Predicted Mid
5 Adiabatic Predicted Mid

0
7/18/2007 0:00 7/18/2007 12:00 7/19/2007 0:00 7/19/2007 12:00 7/20/2007 0:00 7/20/2007 12:00 7/21/2007 0:00 7/21/2007 12:00
Date

Figure 99. Predicted pavement temperatures versus measurements (pavement mid, Alma
Center, WI)

Pavement temperature-Alma Center, WI

45

40

35

30
Temperature ( C)
o

25

20

15 Measured Bottom
Isothermal Predicted Bottom
10 Adiabatic Predicted Bottom

0
7/17/2007 19:12 7/18/2007 9:36 7/19/2007 0:00 7/19/2007 14:24 7/20/2007 4:48 7/20/2007 19:12 7/21/2007 9:36

Date

Figure 100. Predicted pavement temperatures versus measurements (pavement bottom,

Alma Center, WI)

114
5.7.2 Atlantic Pavement Temperature and Prediction

5.7.2.1 Inputs

The weather information for temperature, wind speed and humidity in Atlantic, Iowa is plotted in
Figure 101–103.

Temperature-Atlantic, IA
85

80

75
Temperature ( C)
o

70

65

60

55

50
6/27/07 9:36 6/27/07 13:12 6/27/07 16:48 6/27/07 20:24 6/28/07 0:00 6/28/07 3:36 6/28/07 7:12 6/28/07 10:48
Date

Figure 101. Temperature in Atlantic, IA

115
 Wind speed-Atlantic, IA
10

7
Wind speed (mile/hr)

0
6/27/07 9:36 6/27/07 13:12 6/27/07 16:48 6/27/07 20:24 6/28/07 0:00 6/28/07 3:36 6/28/07 7:12 6/28/07 10:48
Date

Figure 102. Wind Speed in Atlantic, IA

Humidity-Atlantic, IA
80

70
Humidity (%)

60

50

40

30
6/27/07 9:36 6/27/07 13:12 6/27/07 16:48 6/27/07 20:24 6/28/07 0:00 6/28/07 3:36 6/28/07 7:12 6/28/07 10:48
Date

Figure 103. Humidity in Atlantic, IA

116
5.7.2.2 Results and Analysis

The predicted temperatures of pavement placed in Atlantic, Iowa are presented in Figure 104–
106. The results of hydration curve parameters modeled by semi-adiabatic test data match actual
pavement temperatures better than the hydration curve parameters resulting from isothermal test
data. It is noted that the pavement temperatures for the bottom of the slab experienced a sharp
drop which might be attributed to sensor error during that period.

Figure 104. Predicted pavement temperatures versus measurements (pavement top,

Atlantic, IA)

117
Figure 105. Predicted pavement temperatures versus measurements (pavement mid,
Atlantic, IA)

Figure 106. Predicted pavement temperatures versus measurements (pavement mid,

Atlantic, IA)

118
5.7.3 Ottumwa Pavement Temperature and Prediction

5.7.3.1 Inputs

The weather information of temperature, wind speed and humidity in Ottumwa, Iowa were
downloaded from the Weather Underground website (http://www.wunderground.com/) and are
shown in Figure 107–109.

Temperature-Ottumwa, IA
100

96

92

88
Temperature ( C)

84
o

80

76

72

68

64

60
7/23/2007 19:12 7/24/2007 12:00 7/25/2007 4:48 7/25/2007 21:36 7/26/2007 14:24 7/27/2007 7:12 7/28/2007 0:00 7/28/2007 16:48

Date

Figure 107. Temperature in Ottumwa, IA

119
 Wind Speed-Ottumwa, IA
10

8
Wind speed (mile/hr)

0
7/23/2007 19:12 7/24/2007 12:00 7/25/2007 4:48 7/25/2007 21:36 7/26/2007 14:24 7/27/2007 7:12 7/28/2007 0:00 7/28/2007 16:48
Date

Figure 108. Wind speed in Ottumwa, IA

Humidity-Ottumwa, IA
100

90

80

70

60
Humidity (%)

50

40

30

20

10

0
7/23/2007 19:12 7/24/2007 12:00 7/25/2007 4:48 7/25/2007 21:36 7/26/2007 14:24 7/27/2007 7:12 7/28/2007 0:00 7/28/2007 16:48
Date

Figure 109. Humidity in Ottumwa, IA

5.7.3.2 Results and Analysis

The predicted temperatures of a pavement in Ottumwa using both the hydration curve parameters
back-calculated from the isothermal test and the semi-adiabatic test are presented in Figures
110–112. Like the cases before, the results indicate hydration curve parameters resulting from
semi-adiabatic test data (as opposed to isothermal test data) are a better match to actual pavement
temperatures. As seen in the previous case, a sharp drop in actual pavement temperatures is

120
recorded for the bottom of the slab. Again, this drop could be attributed to sensor error.

Pavement temperature-Ottumwa, IA
50

45

40

35
Temperature ( C)

30
o

25

20 Measured Top
Adiabatic Predicted Top
15
Isothermal Predicted Top

10

0
7/23/2007 19:12 7/24/2007 9:36 7/25/2007 0:00 7/25/2007 14:24 7/26/2007 4:48 7/26/2007 19:12 7/27/2007 9:36 7/28/2007 0:00
Date

Figure 110. Predicted pavement temperatures versus measurements (pavement top,

Ottumwa, IA)

Pavement temperature-Ottumwa, IA
50

45

40

35
Temperature ( C)

30
o

25

20
Measuerd Mid
15 Aidabatic Predicted Mid
Isothermal Predicted Mid
10

0
7/23/2007 19:12 7/24/2007 9:36 7/25/2007 0:00 7/25/2007 14:24 7/26/2007 4:48 7/26/2007 19:12 7/27/2007 9:36 7/28/2007 0:00
Date

Figure 111. Predicted pavement temperatures versus measurements (pavement mid,

Ottumwa, IA)

121
 Pavement temperature-Ottumwa, IA
50

45

40
Temperature ( C)

35
o

30

Measured Bottom
25
Aidabatic Predicted Bottom
Isothermal Predicted Bottom
20

15

10
7/24/2007 0:00 7/24/2007 12:00 7/25/2007 0:00 7/25/2007 12:00 7/26/2007 0:00 7/26/2007 12:00 7/27/2007 0:00 7/27/2007 12:00 7/28/2007 0:00
Date

Figure 112. Predicted pavement temperatures versus measurements (pavement bottom,

Ottumwa, IA)

5.7.4 Summary

In summary of this section, the predicted pavement temperatures using HIPERPAV software
prove to be in agreement with actual measurements. The simulated temperatures using the
hydration curve parameters of semi-adiabatic tests were proven to have higher accuracy than
those using the hydration curve parameters of isothermal tests. This result could be attributed to
at least two reasons: (1) the semi-adiabatic test condition of increased temperature is closer to
that of the in situ pavement than that of isothermal test condition of constant temperature; (2) the
isothermal test in this project is performed on the cement mortar, while the semi-adiabatic test is
performed on concrete as that of in situ pavement. Therefore, the hydration curve parameters of
semi-adiabatic tests are recommended for implementation in HIPERPAV software.

5.8 Conclusion

This section presented procedures for ascertaining hydration curve parameters from isothermal
and semi-adiabatic calorimetric test data in an effort to create a modified version of Federal
Highway’s HIPERPAV II software that would predict concrete hydration and pavement
temperatures with more accuracy. Several analyses were also performed to establish which set of
parameters from laboratory testing (isothermal or semi-adiabatic) offer better accuracy in
HIPERPAV analysis of actual field testing sites.

The original HIPERPAV II software uses an embedded, empirical, chemical-based function

(6,7,8) to determine hydration curve parameters to develop heat evolution. However, it would be
more reliable to use laboratory or field test results to characterize the hydration of cementitious
materials. First, the activation energy, a material parameter necessary for determining hydration

122
curve parameters, was computed using the Arrhenius equation. Hydration curve parameters were
calculated using both the isothermal and semi-adiabatic test data for the rate of heat evolution. A
mathematical model and computation approach to convert the isothermal calorimetry of cement
mortar to semi-adiabatic calorimetric of cement concrete was developed and realized using the
finite difference method. The HIPERPAV II software was modified to allow user defined inputs
for hydration curve parameters. Finally, analyses using the modified software (for both
isothermal and semi-adiabatic data inputs) were compared to actual field site conditions and
pavement temperatures at three different locations.

As a result of the comparison, it was determined that a higher accuracy could be achieved in
HIPERPAV analyses by using hydration curve parameters calculated from semi-adiabatic test
data.

It is critical to predict pavement temperature effectively in order to evaluate the development of

critical stresses and concrete strengths when using the HIPERPAV software. Therefore,
hydration curve parameters based on the semi-adiabatic tests are recommended as inputs to the
software for increased accuracy and reliability. Already a powerful tool for the paving
community, an even more accurate and reliable HIPERPAV program will give contractors that
much more of an edge on predicting early age concrete behavior, preventing unnecessary
cracking, and securing their financial investments.

123
6. SPECIFICATION MODIFICATION

During the phase III study, the isothermal calorimetry tests followed the procedure described in
the draft of a specification developed in the phase II study. Minor modifications were made on
the test procedure during the phase III field tests. The revised specification for the isothermal
calorimeter equipment and test method for mortar and concrete is presented in Appendix E. It is
expected that the proposed specification of the present research will serve as a key reference for
the future ASTM and/or AASHTO concrete calorimeter specification development.

124
7. CONCLUSIONS AND RECOMMENDATIONS

Three field sites, US 71 (Atlantic, Iowa), Highway 95 (Alma Center, Wisconsin), and US 63
bypass (Ottumwa, Iowa) were selected, and calorimetry tests were conducted at these field sites
using different calorimeters: a simple isothermal calorimeter, and two semi-adiabatic
calorimeters (AdiaCal and IQ drum). The set times of the field concrete were also measured
according to ASTM C403, and general properties of the concrete and pavement (such as concrete
slump, air content, unit weight, w/c, placement temperature, and pavement subbase temperature
and sawing time) were also recorded. The results from the field tests indicate the following:
• AdiaCal semi-adiabactic calorimetry tests, using concrete samples, can provide general
information on concrete performance. The test results are very sensitive to the concrete
placement temperature. (The temperature curves obtained from the AdiaCal calorimeter tests
varied largely in the samples tested in the same day.) Thus, the test results are useable for set
time prediction of field concrete but not desirable for accurate quality control.
• Same as the finding drawn in the phase II study, the thermal set times obtained form both
AdiaCal and isothermal calorimetry tests are well related to those from the ASTM C403
tests. Compared with the isothermal calorimetry test, the AdiaCal test is easy to operate.
• The simple isothermal calorimetry test results of samples at a given project were consistent.
The test results of samples from different projects looked very different, demonstrating the
subtle changes in these concrete materials and/or mixture proportions. As a result, the simple
isothermal calorimeter could be a good tool for daily concrete quality control.
• In the simple isothermal calorimetry tests, concrete samples showed much larger variations
than mortar samples. Therefore, mortar samples sieved from field concrete are recommended
for field calorimetry tests.
• The general property tests of field concrete (such as slump, temperature, air content, and unit
weight and w/c tests) indicated that field concrete mixes were consistent from day to day. No
incompatibility problem was identified in the concrete studied.
• Neither the isothermal calorimeter nor AdiaCal showed good ability to identify changes in
w/c ratio of the field concrete. Hence, the microwave method can be used as a supplementary
test for such identification.
• Pavement sawing times were close to the final setting time in these three field projects, but
no clear relationship was observed between the setting and sawing times.

Robust tests were conducted in lab for the concrete materials obtained from the above mentioned
three field sites. Nine robust mixes, with 50% decrease/increase of WR and/or FA dosages were
developed based on the mix proportion actually used in field for each field project. AdiaCal tests
were performed for each robust mix, and isothermal calorimeter tests were performed for each
robust mix at four different temperatures. Selected IQ drum tests and ASTM C403 set time tests
were also performed in lab so as to compare the lab results with the field test results. A statistical
analysis was conducted to analyze these test data. The results from the lab tests for the field
materials suggest the following:
• The results from the lab tests for the field materials are generally consistent with those from
the corresponding field tests.
• The simple isothermal tests showed clearly a second peak related to the hydration of fly ash
in the concrete mixes tested. Such a heat evolution peak was not generally observed from

125
 AdiaCal or IQ Drum tests.
• The thermal set times obtained from both AdiaCal and isothermal calorimetry tests were
closely related to those from the ASTM C403 tests. The effects of WR dosage and FA
replacement level on concrete set time could be identified by both calorimetry test methods.
• The simple isothermal test results illustrated that as testing temperature increased, the
variation in thermal set time decreased. This implies that potential concrete set time and
strength development problems might show in winter construction while fewer problems
may be expected in summer construction.
• Testing/curing temperature had a more significant effect on concrete calorimetry parameters
(thermal set time and the area under the heat evolution curve) than WR and FA.
• Compared with FA, WR has less effect on thermal set time. However, in a different project,
WR affected calorimetry parameters differently.
• The robust tests demonstrated that when the WR and/or FA amounts are 50% higher or lower
than the designed dosage, the concrete heat-generation curves looked similar but shifted only
to the left or right, depending upon the degree of material variation. There was no
incompatibility problem within these mixes tested at the designed testing temperature.
• The robust test method can be used for establishing acceptable heat evolution boundaries.
Thus, field engineers can easily evaluate their calorimetry test results and use the calorimetry
as a single tool for field concrete quality control.

The computation and theoretical modeling are performed for ascertaining hydration curve
parameters from isothermal and semi-adiabatic calorimetric test data, in an effort to create a
modified version of Federal Highway’s HIPERPAV II software that would predict concrete
hydration and pavement temperatures with more accuracy. The original HIPERPAV II software
is modified to allow the users to input the laboratory or field-test determined hydration curve
parameters. First, the activation energy, a material parameter necessary for determining
hydration curve parameters, was computed using the Arrhenius equation. Consequently,
hydration curve parameters were calculated using both the isothermal and semi-adiabatic test
data. Meanwhile, a mathematical model and computation approach to convert the isothermal
calorimetry of cement mortar to semi-adiabatic calorimetry of cement concrete was developed
and realized using the finite difference method. Finally, analyses using the modified software
(for both isothermal and semi-adiabatic data inputs) were compared to actual field site conditions
and pavement temperatures at three different locations (Alma Center, WI; Atlantic, IA;
Ottumwa, IA). The primary findings are summarized as the following:
• The computed activation energies of cementitioius materials used in this research from the
isothermal test data are close to the values reported by other researchers; adding WR and FA
replacement seems to improve activation energy to some extent
• A higher accuracy of predicted pavement temperatures could be achieved in HIPERPAV
analyses by using hydration curve parameters calculated from semi-adiabatic test data.
• It is critical to predict pavement temperature effectively in order to evaluate the development
of critical stresses and concrete strengths using the HIPERPAV software. Therefore,
hydration curve parameters based on the semi-adiabatic tests are recommended as inputs to
the software for increased accuracy and reliability.
• The simulated semi-adiabatic temperatures converted from the isothermal heat signatures
using the theoretical models seem to have a reasonable agreement with the measurements
though there is some small delay at the early stage. Therefore, it is a possibility to use this

126
 model and computation approach for conversion between different calorimetry signatures.

Based on the results of the present study, the following recommendations are proposed:
• Calorimetry tests may be used (1) by concrete mix proportion designers and the cement
industry for checking strength development at different temperature condition and the
incompatibility of using SCMs and chemical admixtures, (2) by contractors as a quality
control tool for flagging material changes and mix proportion errors and for estimation of
concrete set time (AdiaCal tests), and (3) by others for prediction concrete pavement
temperature development and cracking potential via using the HIPERPAV.program.
• The calorimetry research results shall be disseminated through various workshops, tech
notes, newsletters, and websites to increase awareness of advantages of using calorimetry in
concrete practice.
• Research should be continued on the specification development for using calorimetry
technique in concrete and on the prediction of concrete performance using calorimetry test
results in the HIPERPAV program.

127
8. REFERENCES

1 Portland Cement Association. Portland Cement, Concrete, and Heat of Hydration.

Concrete Technology Today. Vol. 18, 2.

2 Knight, G. Comparative Calorimetry Testing. Presented at the Technical Working Group

Meeting for the Heat Evolution Test Research. Des Moines, Iowa : s.n., Oct. 1, 2004.

3 K. Wang, Z. Ge, J. Grove, J. M. Ruiz, R. Rasmussen, and T. Ferragut. Developing a

Simple and Rapid Test for Monitoring the Heat Evolution of Concrete Mixtures for Both
Laboratory and Field Applications. Ames, Iowa : Center for Transportation Research and
Education, 2007.

4 Midess, S, Young, J.F. and Darwin, D. Concrete. Prentice Hall, NJ, 2003.

5 FHWA and Iowa State University.

http://www.cptechcenter.org/publications/task15/task15.cfm. [Online] Jan. 2008

6 McCullough, B.F. and Rasmussen, Robert O., “Fast-Track Paving: Concrete Temperature
Control and Traffic Opening Criteria for Bonded Concrete Overlays – Volume I: Final
Report,” Federal Highway Administration Report FHWA-RD-98-167, Washington,
1999.

7 Ruiz, J. M., Rasmussen, R. O., Chang, G. K., Dick, J. C., Nelson, P. K., Ferragut, T. R.,
“Computer-Based Guidelines for Concrete Pavements, Volume I: Project Summary,”
Publication No. FHWA-HRT-04-121, McLean, VA, February 2005.

8 Ruiz, J. M., Rasmussen, R. O., Chang, G. K., Dick, J. C., Nelson, P. K., “Computer-
Based Guidelines for Concrete Pavements, Volume II: Design and Construction
Guidelines and HIPERPAV® II User’s Manual,” Publication No. FHWA-HRT-04-122,
McLean, VA, February 2005.

9 Ruiz, J. M., Rasmussen, R. O., Chang, G. K., Dick, J. C., Nelson, P. K., “Computer-
Based Guidelines for Concrete Pavements,” Volume III: Technical Appendices,
Publication No. FHWA-HRT-04-127, McLean, VA, February 2005.

10 Poole, J. L., Riding, K. A., Folliard, K. J., Juenger, M.C.G., and Schindler, A.K.,
“Methods for Calculating Activation Energy for Portland Cement,” ACI Materials
Journal, V. 104, No. 1, January-February 2007.

11 Schindler, A.K., “Effect of Temperature on Hydration of Cementitious Materials,” ACI

Materials Journal, V. 101, No.1, 2004

12 Wadsö, L., “An experimental comparison between isothermal calorimetry, semi adiabatic
calorimetry and solution calorimetry for the study of cement hydration,” final report,
NORDTEST project 1534-01, 2002.

128
13 Tank , R.C., “The rate constant model for strength development of concrete,” Ph.D.
dissertation, Polytechnic University, Brooklyn, New York, June 1988.

14 Freiesleben Hansen, P., and Pedersen, E.J., “Maturity Computer for Controlling. Curing
and Hardening of Concrete,” Nordisk Betong, Vol.19, 21-25, 1977.

129
APPENDIX A: INFORMATION OF FIELD PROJECTS

A.1 Information for Atlantic Project

Batch ticket
Date: June 27, 2007 Time: 12:38:26 p.m.
Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 11640 11710 -0.06 554.3 5.00 Dry Aggs 26678
CA 13420 13353 0.50 93.3 0.70 Cemes 4695
IA 2300 2355 -2.30 34.0 1.50 Waters 1932
Cement 3760 3757 0.10 Total 33305
Fly Ash 935 935 0.00 w/c 0.411
Water 150 G 153 -2.00 1250.0 Add: -1G
Air Entr 107 fl.oz 108 fl.oz -1.70 Temper: 0G
Reducer 189 fl.oz 188 fl.oz 0.70

Date: June 28, 2007 Time: 9:15:18 a.m.

Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 11680 11710 -0.3 556.2 5.00 Dry Aggs 26657
CA 13340 13353 -0.1 92.7 0.70 Cemes 4685
IA 2320 2355 -1.5 34.3 1.50 Waters 1867
Cement 3750 3757 -0.2 Total 33208
Fly Ash 935 935 0.0 w/c 0.398
Water 125 G 153 -2.3 1041.7 Add: 6G
Air Entr 108 fl.oz 108 fl.oz -2.3 Temper: 17 G
Reducer 187 fl.oz 188 fl.oz -0.4

A-1
Date: June 28, 2007 Time: 11:20:37 a.m.
Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 11660 11710 -0.4 555.2 5.00 Dry aggs 26598
CA 13320 13353 -0.2 92.6 0.70 Cemes 4680
IA 2300 2355 -2.3 34.0 1.50 Waters 1865
Cement 3745 3757 -0.3 Total 33143
Fly Ash 935 935 0.0 w/c 0.399
Water 120 G 153 -2.4 1000.0 Add: 6G
Air Entr 108 fl.oz 108 fl.oz -2.3 Temper: 22 G
Reducer 187 fl.oz 188 fl.oz -0.4

Date: June 28, 2007 Time: 1:37:34 p.m.

Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 11680 11710 -0.3 556.2 5.00 Dry Aggs 26577
CA 13260 13353 -0.7 92.2 0.70 Cemes 4685
IA 2320 2355 -1.5 34.3 1.50 Waters 1949
Cement 3760 3757 0.1 Total 33212
Fly Ash 925 935 -1.1 w/c 0.416
Water 141 G 153 -1.4 1175.0 Add: -4 G
Air Entr 108 fl.oz 108 fl.oz -2.3 Temper: 11 G
Reducer 187 fl.oz 188 fl.oz -0.4

Date: June 29, 2007 Time: 9:07:03 a.m.

Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 11700 11710 -0.2 556.2 5.00 Dry Aggs 26531
CA 13260 13353 -0.8 92.7 0.80 Cemes 4660
IA 2280 2355 -3.3 34.3 1.60 Waters 2009
Cement 3725 3757 -0.9 Total 3320
Fly Ash 9935 935 0.0 w/c 0.431
Water 127 G 153 -2.3 1058.3 Add: -12 G
Air Entr 108 fl.oz 108 fl.oz -2.3 Temper: 29 G
Reducer 187 fl.oz 188 fl.oz -0.4

A-2
Date: June 29, 2007 Time: 10:59:03 a.m.
Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 11740 11710 0.2 569.7 5.00 Dry Aggs 26845
CA 13280 13353 -0.6 105.4 0.80 Cemes 4670
IA 2540 2355 7.7 40.0 1.60 Waters 1948
Cement 3765 3757 0.2 Total 33463
Fly Ash 905 935 -3.2 w/c 0.417
Water 142 G 153 -2.1 1183.3 Add: -5 G
Air Entr 108 fl.oz 108 fl.oz -2.3 Temper: 6G
Reducer 187 fl.oz 188 fl.oz -0.4

Date: June 29, 2007 Time: 2:59:03 p.m.

Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 11740 11710 0.2 569.7 5.10 Dry Aggs 26727
CA 13360 13353 0.0 106.0 0.80 Cemes 4670
IA 2340 2355 -0.7 36.9 1.60 Waters 2013
Cement 3735 3757 -0.6 Total 33410
Fly Ash 935 935 0.0 w/c 0.43
Water 137 G 153 -2.1 1141.7 Add: -12 G
Air Entr 108 fl.oz 108 fl.oz -2.3 Temper: 19 G
Reducer 187 fl.oz 188 fl.oz -0.4

Date: June 30, 2007 Time: 8:53:51 a.m.

Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 13380 13340 0.3 79.8 0.6 Dry Aggs 26800
CA 11740 11698 0.4 548.4 4.9 Cemes 4695
IA 2340 2353 -0.6 32.3 1.4 Waters 1860
Cement 3770 3757 0.3 Total 33355
Fly Ash 925 935 -1.1 w/c 0.396
Water 144 G 146 G -1.4 1200.0 Add: 7G
Air Entr 110 fl.oz 112 fl.oz -2.0 Temper: 0G
Reducer 187 fl.oz 188 fl.oz -0.4

A-3
Date: June 30, 2007 Time: 11:45:41 a.m.
Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 13280 13340 -0.4 79.2 0.60 Dry Aggs 26802
CA 11640 11698 -0.5 543.7 4.90 Cemes 4685
IA 2540 2353 7.9 35.1 1.40 Waters 1966
Cement 3765 3757 0.2 Total 33453
Fly Ash 920 935 -1.6 w/c 0.42
Water 148 G 151 G -2.0 1233.3 Add: -6 G
Air Entr 110 fl.oz 112 fl.oz -2.0 Temper: 9G
Reducer 187 fl.oz 188 fl.oz -0.4

Date: June 30, 2007 Time: 1:23:31 p.m.

Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 13400 13340 0.5 79.9 0.60 Dry Aggs 26704
CA 11660 11698 -0.3 544.7 4.90 Cemes 4680
IA 2300 2353 -2.3 31.8 1.40 Waters 2040
Cement 3745 3757 -0.3 Total 33423
Fly Ash 935 935 0.0 w/c 0.436
Water 153 G 146 G -1.9 1275.0 Add: -15 G
Air Entr 111 fl.oz 112 fl.oz -1.1 Temper: 13 G
Reducer 187 fl.oz 188 fl.oz -0.4

Date: July 2, 2007 Time: 9:14:19 a.m.

Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 13240 13287 -0.4 26.4 0.20 Dry Aggs 26566
CA 11540 11620 -0.7 465.1 4.20 Cemes 4685
IA 2300 2344 -1.9 22.8 1.00 Waters 1864
Cement 3770 3757 0.3 Total 33115
Fly Ash 915 935 -2.1 w/c 0.398
Water 162 G 163 G -0.6 1350.0 Add: 6G
Air Entr 111 fl.oz 112 fl.oz -1.1 Temper: 0G
Reducer 187 fl.oz 188 fl.oz -0.4

A-4
Date: July 2, 2007 Time: 10:55:39 a.m.
Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 13240 13287 -0.4 26.4 0.20 Dry Aggs 26546
CA 11520 11620 -0.9 464.3 4.20 Cemes 4710
IA 2300 2344 -1.9 22.8 1.00 Waters 1830
Cement 3765 3757 0.2 Total 33087
Fly Ash 945 935 1.1 w/c 0.389
Water 158 G 158 G 0.0 1316.7 Add: 12 G
Air Entr 112 fl.oz 112 fl.oz -0.2 Temper: 0G
Reducer 187 fl.oz 188 fl.oz -0.4

Date: July 2, 2007 Time: 12:53:42 p.m.

Batch Size: 8,50 cyds
Indication Targets WatFree Moist
Material % Tol (lb)
(lb) (lb) (lb) %
FA 13360 13287 0.6 26.7 0.20 Dry Aggs 26819
CA 11720 11620 0.9 472.4 4.20 Cemes 4720
IA 2260 2344 -3.6 22.4 1.00 Waters 1855
Cement 3780 3757 0.6 Total 33393
Fly Ash 940 935 0.5 w/c 0.393
Water 145 G 148 G -2.0 1208.3 Add: 9G
Air Entr 113 fl.oz 114 fl.oz -0.8 Temper: 15 G
Reducer 188 fl.oz 188 fl.oz 0.2

A-5
Figure A.1. Concrete temperature for all samples for Atlantic project

A-6
A.2 Information for Alma Center Project

Batch Ticket
Date: July 17, 2007 Time: 08:42:11 a.m.
Ticket No. 13575 Truck no.
Batch Size: 10.00 cyds Total Shipped 450.00 cyds
Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water
Sand 1370.00 14043 13940 0.993 2.50% 340.00 40.02
3/4 in. 1210.00 12221 12140 0.993 1.00% 120.20 14.43
1 ½ in. 615.00 6212 6160 0.992 1.00% 60.99 7.32
Cement 446.00 4460 4448 0.997
Fly Ash 113.00 1130 1105 0.978
Water 20.00 2041 1999 0.980 1999.19 240.00
Daravair 5.50 55.0 54.0 0.982 3.51 0.42
WRDA 82 18.00 180.00 177.0 0.983 11.52 1.38
Water Trim 916.30 lb Water 0.00 Total 2535.42 lb 304.37 gal
Added Water
w/c 0.457

Date: July 17, 2007 Time: 10:51:58 a.m.

Ticket No. 13629 Truck no.
Batch Size: 10.00 cyds Total Shipped 10.00 cyds
Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water
Sand 1370.00 14043 13980 0.996 2.50% 340.98 40.93
¾ in. 1210.00 12221 12160 0.995 1.00% 120.40 14.45
1 ½ in. 615.00 6212 6240 1.005 1.00% 61.78 7.42
Cement 750.00 7500 7437 0.992
Fly Ash 0.00 0 0 0
Water 25.00 2416 2374 0.983 2374.05 285.00
Daravair 6.75 68 68.0 1.00 4.43 0.53
WRDA 82 22.50 225 222.0 0.987 14.45 1.73
Water Trim 874.65 lb Water 0.00 Total 2916.08 lb 350.07 gal
Added Water
w/c 0.392

A-7
Date: July 17, 2007 Time: 01:28:35 p.m.
Ticket No. 13689 Truck no.
Batch Size: 10.00 cyds Total Shipped 1580.00 cyds
Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water
Sand 1370.00 14043 13960 0.994 2.50% 340.49 40.87
¾ in. 1210.00 12221 12180 0.997 1.00% 120.59 14.48
1 ½ in. 615.00 6212 6140 0.988 1.00% 60.79 7.30
Cement 446.00 4460 4431 0.993
Fly Ash 113.00 1130 1144 1.012
Water 20.00 1999 1958 0.979 1957.55 235.00
Daravair 6.50 65 65.0 1.000 4.23 0.51
WRDA 82 18.00 180 177.0 0.983 11.52 1.38
Water Trim 874.65 lb Water 0.00 Total 2495.17 lb 299.54 gal
Added Water
w/c 0.448

Date: July 17, 2007 Time: 02:59:25 p.m.

Ticket No. 13725 Truck no.
Batch Size: 10.00 cyds Total Shipped 1940.00 cyds
Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water
Sand 1370.00 14043 14120 1.005 2.50% 344.39 41.34
¾ in. 1210.00 12221 12100 0.990 1.00% 119.80 14.38
1 ½ in. 615.00 6212 6240 1.005 1.00% 61.78 7.42
Cement 446.00 4460 4427 0.993
Fly Ash 113.00 1130 1124 0.995
Water 20.00 1999 1958 0.979 1957.55 235.00
Daravair 6.00 60.0 60.0 1.000 3.90 0.47
WRDA 82 18.00 180.00 177.0 0.983 11.52 1.38
Water Trim 874.65 lb Water 0.00 Total 2498.35 lb 299.99 gal
Added Water
w/c 0.450

A-8
Date: July 18, 2007 Time: 09:23:48 a.m.
Ticket No. 13804 Truck no.
Batch Size: 10.00 cyds Total Shipped 670.00 cyds
Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water
Sand 1370.00 14043 13940 0.993 2.50% 340.00 40.02
¾ in. 1210.00 12221 12220 1.000 1.00% 120.99 14.52
1 ½ in. 615.00 6212 6100 0.920 1.00% 60.40 7.25
Cement 446.00 4460 4450 0.998
Fly Ash 113.00 1130 1089 0.964
Water 20.00 1974 1933 0.979 1932.56 232.00
Daravair 6.50 65.0 65 1.000 4.23 0.51
WRDA 82 18.00 180 177 0.983 11.52 1.38
Water Trim 853.82 lb Water 0.00 Total 22469.7lb 296.48 gal
Added Water
w/c 0.446

Date: July 18, 2007 Time: 10:47:14 a.m.

Ticket No. 13840 Truck no.
Batch Size: 10.00 cyds Total Shipped 1030.00 cyds

Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water

Sand 1370.00 14043 14060 1.001 2.50% 342.93 41.17
¾ in. 1210.00 12221 12120 0.992 1.00% 120.00 14.41
1 ½ in. 615.00 6212 6260 1.000 1.00% 61.98 7.44
Cement 446.00 4460 4427 0.993
Fly Ash 113.00 1130 1149 1.017
Water 20.00 1999 1958 0.979 1957.55 235.00
Daravair 6.50 65 65.0 1.000 4.23 0.51
WRDA 82 18.00 180 177 0.983 11.52 1.38

Water Trim 874.65 lb Water 0.00 Total 2498.21 lb 299.90 gal

Added Water
w/c 0.448

A-9
Date: July 18, 2007 Time: 2:07:46 p.m.
Ticket No. 13922 Truck no.
Batch Size: 10.00 cyds Total Shipped 1850.00 cyds

Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water

Sand 1370.00 14043 13980 0.996 2.50% 340.98 40.93
¾ in. 1210.00 12221 12100 0.990 1.00% 119.80 14.38
1 ½ in. 615.00 6212 6220 1.001 1.00% 61.58 7.39
Cement 446.00 4460 4417 0.990
Fly Ash 113.00 1130 1126 0.996
Water 20.00 2041 1999 0.980 1999.19 240.00
Daravair 6.50 65 65 1.000 4.23 0.51
WRDA 82 18.00 180 177 0.983 11.52 1.38

Water Trim 916.30 lb Water 0.00 Total 2537.31 lb 304.60 gal

Added Water
w/c 0.458

Date: July 18, 2007 Time: 3:07:51 p.m.

Ticket No. 13943 Truck no.
Batch Size: 10.00 cyds Total Shipped 2050.00 cyds

Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water

Sand 1370.00 14043 13980 0.996 2.50% 340.98 40.93
¾ in. 1210.00 12221 12200 0.998 1.00% 120.79 14.50
1 ½ in. 615.00 6212 6100 0.982 1.00% 60.40 7.25
Cement 446.00 4460 4430 0.993
Fly Ash 113.00 1130 1126 0.996
Water 20.00 1999 1958 0.979 1957.55 235.00
Daravair 6.50 65 64 0.985 4.17 0.50
WRDA 82 18.00 180 177 0.983 11.52 1.38

Water Trim 874.65 lb Water 0.00 Total 2495.40 lb 299.57 gal

Added Water
w/c 0.449

A-10
Date: July 19, 2007 Time: 08:59:33 a.m.
Ticket No. 13992 Truck no.
Batch Size: 10.00 cyds Total Shipped 490.00 cyds

Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water

Sand 1370.00 14043 14120 1.005 2.50% 344.39 41.34
¾ in. 1210.00 12221 12160 0.995 1.00% 120.40 14.45
1 ½ in. 615.00 6212 6220 1.001 1.00% 61.58 7.39
Cement 446.00 4460 4417 0.990
Fly Ash 113.00 1130 1144 1.012
Water 20.00 2016 1933 0.979 1932.56 232.00
Daravair 6.50 65 60.0 1.000 3.90 0.47
WRDA 82 18.00 180 177 0.983 11.52 1.38

Water Trim 853.83 lb Water 0.00 Total 2474.35 lb 297.04 gal

Added Water
w/c 0.445

Date: July 19, 2007 Time: 10:31:07 a.m.

Ticket No. 14030 Truck no.
Batch Size: 10.00 cyds Total Shipped 870.00 cyds

Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water

Sand 1370.00 14043 14000 0.997 2.50% 341.46 40.99
¾ in. 1210.00 12221 12140 0.993 1.00% 120.20 14.43
1 ½ in. 615.00 6212 6220 1.001 1.00% 61.58 7.39
Cement 446.00 4460 4421 0.991
Fly Ash 113.00 1130 1134 1.004
Water 20.00 2016 1958 0.979 1957.55 235.00
Daravair 6.50 65 59 0.983 3.54 0.46
WRDA 82 18.00 180 177 0.983 11.52 1.38

Water Trim 874.65 lb Water 0.00 Total 2496.15 lb 299.66 gal

Added Water
w/c 0.449

A-11
Date: July 19, 2007 Time: 11:54:39 a.m.
Ticket No. 14047 Truck no.
Batch Size: 10.00 cyds Total Shipped 1040.00 cyds

Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water

Sand 1370.00 14043 14000 0.997 2.50% 341.46 40.99
¾ in. 1210.00 12221 12140 0.993 1.00% 12.20 14.43
1 ½ in. 615.00 6212 6240 1.005 1.00% 61.78 7.42
Cement 446.00 4460 4429 0.993
Fly Ash 113.00 1130 1136 1.005
Water 20.00 2016 1974 0.979 1974.20 237.00
Daravair 6.50 65 60 1.000 3.90 0.47
WRDA 82 18.00 180 177 0.983 11.52 1.38

Water Trim 895.47 lb Water 0.00 Total 2513.08 301.69 gal

Added Water
w/c 0.452

Date: July 19, 2007 Time: 01:55:39 p.m.

Ticket No. 14097 Truck no.
Batch Size: 10.00 cyds Total Shipped 1530.00 cyds

Material Dsg Qty Req’d Bat’d B/R Moisture Actual Water

Sand 1370.00 14043 13960 0.994 2.50% 340.49 lb 40.87 gal
¾ in. 1210.00 12221 12180 0.997 1.00% 120.59 14.48
1 ½ in. 615.00 6212 6300 1.014 1.00% 62.38 7.49
Cement 446.00 4460 4478 1.004
Fly Ash 113.00 1130 1089 0.964
Water 20.00 2016 1974 0.979 1974.20 237.00
Daravair 6.50 65 65 1.000 4.23 0.51
WRDA 82 18.00 180 177 0.983 11.52 1.38

Water Trim 895.47 lb Water 0.00 Total 2513.42 lb 301.73 gal

Added Water
w/c 0.451

A-12
Figure A.2. Concrete temperature for all samples for Alma Center project

A-13
A.3 Information for Ottumwa Project

Batch Ticket
Date: July 24, 2007 Time: 8:30 a.m.
Ticket No. 79 Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 14888 0.5 Water 174 (gal)
Sand 12820 3.0 Tempee water 7 (gal)
Cement 4050 Total Water 1956 (lb)
Fly Ash 1005 w/c 0.387
AEA 97 oz
WR 207 oz

Date: July 24, 2007 Time: 10:13 a.m.

Ticket No. 143 Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 14940 0.5 Water 175 (gal)
Sand 12820 3.0 Tempee water 0 (gal)
Cement 4055 Total Water 1906 (lb)
Fly Ash 990 w/c 0.378
AEA 95 oz
WR 204 oz

Date: July 25, 2007 Time: 8:33 a.m.

Ticket No. Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 16240 0.2 Water 164 (gal)
Sand 12000 3.2 Tempee water 8 (gal)
Cement 3975 Total Water 1838 (lb)
Fly Ash 1005 w/c 0.369
AEA 79 oz
WR 201 oz

Date: July 25, 2007 Time: 9:58 a.m.

Ticket No. Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 16220 0.5 Water 164 (gal)
Sand 11980 3.0 Tempee water 8 (gal)
Cement 4000 Total Water 1838 (lb)
Fly Ash 1005 w/c 0.367
AEA 79 oz
WR 201 oz

A-14
Date: July 25, 2007 Time: 12:30 p.m.
Ticket No. 202 Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 16220 0.2 Water 165 (gal)
Sand 11960 3.2 Tempee water 0 (gal)
Cement 3970 Total Water 1785 (lb)
Fly Ash 985 w/c 0.360
AEA 79 oz
WR 201 oz

Date: July 25, 2007 Time: 1:56 p.m.

Ticket No. 242 Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 16220 0.5 Water 160 (gal)
Sand 12000 3.0 Tempee water 4 (gal)
Cement 3985 Total Water 1770 (lb)
Fly Ash 987 w/c 0.356
AEA 79 oz
WR 201 oz

Date: July 30, 2007 Time: 8:16 a.m.

Ticket No. 65 Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 16280 0.5 Water 155 (gal)
Sand 11940 3.1 Tempee water 8 (gal)
Cement 3965 Total Water 1798 (lb)
Fly Ash 980 w/c 0.364
AEA 97 oz
WR 198 oz

Date: July 30, 2007 Time: 9:32 a.m.

Ticket No. 109 Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 16260 0.5 Water 155 (gal)
Sand 11940 3.1 Tempee water 4 (gal)
Cement 3970 Total Water 1764 (lb)
Fly Ash 980 w/c 0.356
AEA 97 oz
WR 201 oz

A-15
Date: July 30, 2007 Time: 1:37 p.m.
Ticket No. 195 Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 16320 0.5 Water 154 (gal)
Sand 12000 3.1 Tempee water 10 (gal)
Cement 4000 Total Water 1808 (lb)
Fly Ash 1000 w/c 0.362
AEA 97 oz
WR 201 oz

Date: July 30, 2007 Time: 3:15 p.m.

Ticket No. 242 Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 16300 0.5 Water 164 (gal)
Sand 11920 3.1 Tempee water 10gal)
Cement 3970 Total Water 1889 (lb)
Fly Ash 990 w/c 0.381
AEA 97 oz
WR 198 oz

Date: July 31, 2007 Time: 8:47 a.m.

Ticket No. 90 Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 16360 0.2 Water 159 (gal)
Sand 11940 3.1 Tempee water 10 (gal)
Cement 3985 Total Water 1800 (lb)
Fly Ash 980 w/c 0.363
AEA 79 oz
WR 198 oz

Date: July 31, 2007 Time: 10:51 a.m.

Ticket No. 109 Load: 9 yd
Materials Qty (lb) Moisture (%) Materials Qty
Rock 16280 0.2 Water 165 (gal)
Sand 11980 3.1 Tempee water 4 (gal)
Cement 3990 Total Water 1800 (lb)
Fly Ash 1010 w/c 0.360
AEA 79 oz
WR 198 oz

A-16
Figure A.3. Concrete temperature for all samples for Ottumwa project

A-17
APPENDIX B. ADIACAL MORTAR ROBUST TEST RESULTS SUMMARY

Table B.1. Summary of AdiaCal robust test results of US 71 (Atlantic, IA) mixes
Peak
FS- temp, Peak
o
IS, h FS, h IS, h C slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h
1 12.90 21.10 8.20 27.30 0.605 107.0 132.00 149.00 162.00 551.00 559.00
2 14.60 20.90 6.20 28.40 0.745 108.0 133.00 151.00 168.00 561.00 589.00
3 12.30 19.60 7.30 28.60 0.726 110.0 139.00 160.00 170.00 578.00 586.00
4 19.60 21.80 2.20 26.40 0.737 106.0 128.00 138.00 155.00 527.00 552.00
5 10.90 20.80 9.90 27.40 0.711 106.0 136.00 156.00 163.00 561.00 560.00
6 19.70 21.80 2.10 26.60 0.839 106.0 128.00 138.00 156.00 528.00 564.00
7 11.20 20.70 9.50 27.90 0.766 105.0 135.00 157.00 166.00 562.00 574.00
8 18.20 20.20 2.00 26.90 0.737 105.0 130.00 147.00 160.00 542.00 560.00
9 9.50 19.80 10.30 27.60 0.786 105.0 141.00 161.00 165.00 571.00 567.00
Max 19.70 21.80 10.32 28.60 0.839 110.0 141.00 161.00 170.00 578.00 589.00
Min 9.50 19.60 1.98 26.40 0.605 105.0 128.00 138.00 155.00 527.00 552.00
Avg. 14.30 20.70 6.40 27.50 0.739 106.0 133.00 151.00 163.00 553.00 568.00
σ 3.90 0.80 3.48 0.80 0.063 1.70 4.50 8.50 5.10 17.90 12.60
σ% 27.51 3.80 54.38 2.78 8.520 1.56 3.38 5.64 3.12 3.24 2.22

Table B.2. Summary of AdiaCal robust test results of HW 95 (Alma Center, WI) mixes
Peak
FS- temp, Peak A24-
o
IS, h FS, h IS, h C slope A1-6h A6-12h A12-18h A18-24h A1-24h 48h
1 14.10 19.60 5.57 26.90 0.783 108.0 133.00 152.00 160.00 553.00 578.0
2 11.80 20.50 8.70 27.10 0.634 107.0 136.00 154.00 161.00 558.00 578.0
3 12.10 19.60 7.51 27.10 0.729 109.0 141.00 159.00 161.00 569.00 573.0
4 18.30 21.30 2.98 26.10 0.852 111.0 132.00 139.00 155.00 538.00 589.0
5 14.20 20.20 6.04 28.60 0.689 112.0 140.00 160.00 170.00 581.00 596.0
6 20.50 23.60 3.13 25.80 0.822 110.0 130.00 132.00 149.00 521.00 586.0
7 14.30 20.90 6.65 28.50 0.724 111.0 136.00 154.00 170.00 571.00 598.0
8 19.30 23.00 3.78 27.00 0.754 105.0 128.00 138.00 157.00 529.00 595.0
9 13.00 20.70 7.73 29.00 0.771 106.0 137.00 161.00 173.00 576.00 600.0
Max 20.50 23.60 8.70 29.00 0.852 112.0 141.00 161.00 173.00 581.00 600.0
Min 11.80 19.60 2.98 25.80 0.634 105.0 128.00 132.00 149.00 521.00 573.0
Avg. 15.30 21.00 5.79 27.30 0.751 109.0 135.00 150.00 162.00 555.00 588.0
σ 3.20 1.40 2.09 1.10 0.066 2.30 4.20 10.60 7.80 21.60 10.0
σ % 21.14 6.67 36.21 4.03 8.840 2.15 3.14 7.08 4.81 3.89 1.7

B-1
Table B.3. Summary of AdiaCal robust test results of US 63 bypass (Ottumwa , IA) mixes
Peak
FS- temp, Peak
o
IS, h FS, h IS, h C slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h
1 12.15 15.40 3.20 26.90 0.946 103.00 136.00 159.00 154.00 552.00 546.00
2 14.27 17.50 3.20 26.50 0.951 102.00 128.00 152.00 155.00 537.00 547.00
3 11.35 14.80 3.40 27.00 0.909 102.00 140.00 160.00 153.00 555.00 535.00
4 12.48 14.80 2.40 26.60 1.079 104.00 135.00 157.00 151.00 547.00 539.00
5 9.08 14.00 5.00 28.30 1.012 109.00 150.00 168.00 155.00 581.00 547.00
6 14.14 16.50 2.40 26.20 0.830 108.00 133.00 152.00 150.00 543.00 548.00
7 10.63 15.40 4.80 27.60 0.975 107.00 140.00 163.00 154.00 565.00 547.00
8 11.68 13.90 2.20 27.50 0.878 109.00 147.00 162.00 151.00 568.00 545.00
9 8.28 13.20 5.00 30.40 1.256 111.00 164.00 179.00 167.00 621.00 587.00
Max 14.30 17.50 4.97 30.40 1.256 111.00 164.00 179.00 167.00 621.00 587.00
Min 8.30 13.20 2.18 26.20 0.830 102.00 128.00 152.00 150.00 537.00 535.00
Avg. 11.60 15.10 3.50 27.50 0.982 106.00 141.00 161.00 154.00 563.00 549.00
σ 2.00 1.30 1.14 1.30 0.126 3.50 10.90 8.30 5.00 25.80 15.00
σ% 17.59 8.82 32.66 4.64 12.820 3.28 7.68 5.16 3.23 4.580 2.73

B-2
APPENDIX C. ISOTHERMAL MORTAR ROBUST TEST RESULTS SUMMARY

Table C.1. Summary of isothermal robust test results of US 71 (Atlantic, IA) mortar mixes
at 10oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 20.3 29.4 9.1 1.28 0.07 4.2 2.6 3.4 5.5 15.6 27.2 12.9
2 24.1 31.7 7.6 1.26 0.07 4.3 2.4 2.8 4.3 13.8 27.2 14.1
3 17.6 26.8 9.2 1.30 0.08 3.9 3.0 4.5 6.8 18.2 26.9 11.3
4 25.2 31.6 6.4 1.08 0.07 4.3 2.4 2.7 3.9 13.3 24.4 11.0
5 16.5 26.5 10.0 1.40 0.09 3.6 3.2 5.3 7.7 19.8 26.9 13.1
6 28.8 35.1 6.2 1.08 0.07 4.5 2.2 2.2 2.9 11.9 23.4 13.4
7 19.5 29.5 10.0 1.37 0.09 3.8 2.5 3.5 5.9 15.7 28.1 14.5
8 19.4 28.0 8.6 1.11 0.06 4.2 2.6 3.3 5.0 15.2 24.9 9.8
9 14.6 26.2 11.6 1.38 0.09 3.7 3.6 5.9 7.9 21.0 25.8 12.9
Max 28.8 35.1 11.6 1.40 0.09 4.5 3.6 5.9 7.9 21.0 28.1 14.5
Min 14.6 26.2 6.2 1.08 0.06 3.6 2.2 2.2 2.9 11.9 23.4 9.8
Avg. 20.7 29.4 8.7 1.25 0.08 4.1 2.7 3.7 5.5 16.1 26.1 12.5
σ 4.6 2.9 1.8 0.13 0.01 0.3 0.5 1.2 1.7 3.0 1.6 1.6
σ% 22.0 10.0 20.2 10.34 11.48 8.0 16.6 33.0 30.7 19.0 6.0 12.4

Table C.2. Summary of isothermal robust test results of US 71 (Atlantic, IA) mortar mixes
at 20oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 12.2 17.5 5.3 2.43 0.33 3.8 5.7 13.5 12.9 35.9 21.8 NA
2 12.3 18.2 6.0 2.38 0.33 3.5 4.5 12.2 13.0 33.3 22.6 NA
3 11.0 16.8 5.9 2.45 0.35 3.8 6.8 14.2 12.5 37.3 21.1 NA
4 15.8 27.1 11.4 2.30 0.28 4.0 2.6 7.2 12.4 26.2 22.8 NA
5 10.5 14.8 4.2 2.62 0.39 3.5 7.6 15.2 12.6 38.8 23.7 NA
6 19.5 28.6 9.1 2.29 0.27 4.1 2.3 4.7 11.4 22.5 25.2 NA
7 12.5 17.7 5.3 2.72 0.40 3.2 5.5 14.8 14.1 37.5 25.5 NA
8 12.2 24.8 12.6 2.22 0.29 3.4 4.5 11.5 12.4 31.8 19.3 NA
9 9.0 12.4 3.4 2.72 0.40 3.7 11.9 15.3 11.1 42.1 21.6 NA
Max 19.5 28.6 12.6 2.72 0.40 4.1 11.9 15.3 14.1 42.1 25.5 NA
Min 9.0 12.4 3.4 2.22 0.27 3.2 2.3 4.7 11.1 22.5 19.3 NA
Avg. 12.8 19.8 7.0 2.46 0.34 3.7 5.7 12.1 12.5 33.9 22.6 NA
σ 3.1 5.7 3.2 0.19 0.05 0.3 2.9 3.7 0.9 6.3 2.0 NA
σ% 24.4 28.8 46.4 7.59 15.52 8.0 50.6 31.1 7.0 18.5 8.7 NA

C-1
Table C.3. Summary of isothermal robust test results of US 71 (Atlantic, IA) mortar mixes
at 30oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 7.2 10.7 3.5 4.34 1.02 3.9 21.1 19.5 7.1 51.5 NA NA
2 9.3 15.5 6.2 4.39 0.96 3.3 15.2 22.5 7.9 48.9 NA NA
3 6.7 10.1 3.4 4.32 1.08 4.8 22.7 18.2 6.9 52.6 NA NA
4 14.6 15.0 0.4 4.86 1.16 3.5 13.2 20.2 6.7 43.7 NA NA
5 6.7 10.2 3.5 4.63 1.17 4.5 23.9 18.8 8.2 55.3 NA NA
6 15.5 16.1 0.6 4.85 1.02 3.5 8.9 22.3 7.4 42.1 NA NA
7 8.0 11.1 3.1 4.66 1.14 3.4 20.6 21.1 8.7 53.8 NA NA
8 13.9 14.4 0.5 4.78 1.08 3.7 17.4 18.9 6.5 46.5 NA NA
9 6.2 8.4 2.2 4.42 1.17 6.0 24.9 17.1 7.9 55.9 NA NA
Max 15.5 16.1 6.2 4.86 1.17 6.0 24.9 22.5 8.7 55.9 NA NA
Min 6.2 8.4 0.4 4.32 0.96 3.3 8.9 17.1 6.5 42.1 NA NA
Avg. 9.8 12.4 2.6 4.59 1.09 4.1 18.6 19.9 7.5 50.0 NA NA
σ 3.8 2.8 1.9 0.22 0.08 0.9 5.4 1.9 0.7 5.0 NA NA
σ% 38.7 22.9 73.0 4.82 7.09 22.1 28.7 9.3 9.9 10.0 NA NA

Table C.4. Summary of isothermal robust test results of US 71 (Atlantic, IA) mortar mixes
at 40oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 6.4 9.3 2.8 5.17 2.74 6.4 33.3 11.0 7.5 58.2 NA NA
2 6.9 9.7 2.8 6.76 2.72 4.0 32.5 11.7 7.8 56.1 NA NA
3 5.8 8.6 2.8 3.66 2.38 9.3 31.4 9.9 6.9 57.5 NA NA
4 6.8 9.6 2.8 5.85 2.36 4.3 29.4 10.6 7.4 51.7 NA NA
5 5.8 7.0 1.2 4.04 2.82 9.8 33.8 10.7 7.2 61.5 NA NA
6 7.3 10.0 2.7 7.31 2.17 3.3 27.3 11.7 8.0 50.3 NA NA
7 6.6 7.9 1.3 5.54 3.30 5.7 36.0 11.9 7.9 61.4 NA NA
8 6.0 9.1 3.1 4.09 2.25 6.3 29.8 9.6 6.8 52.5 NA NA
9 4.6 6.3 1.7 3.69 0.57 14.7 31.2 10.0 6.7 62.6 NA NA
Max 7.3 10.0 3.1 7.31 3.30 14.7 36.0 11.9 8.0 62.6 NA NA
Min 4.6 6.3 1.2 3.66 0.57 3.3 27.3 9.6 6.7 50.3 NA NA
Avg. 6.2 8.6 2.4 5.12 2.37 7.1 31.6 10.8 7.4 56.8 NA NA
σ 0.8 1.3 0.7 1.35 0.76 3.6 2.6 0.8 0.5 4.6 NA NA
σ% 13.1 15.0 30.9 26.37 32.17 50.8 8.3 7.8 6.6 8.0 NA NA

C-2
Table C.5. Summary of isothermal robust test results of HW 95 (Alma Center, WI) mortar
mixes at 5oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 25.1 34.5 9.4 0.84 0.09 4.0 2.7 2.7 2.9 12.4 18.0 11.9
2 22.1 39.9 17.8 0.72 0.11 4.0 2.0 2.2 2.3 10.6 14.8 13.5
3 21.7 34.4 12.7 0.75 0.10 4.0 2.3 2.3 3.1 11.7 16.6 12.6
4 20.2 45.0 24.8 0.66 0.06 4.0 2.2 2.1 2.2 10.5 12.0 11.6
5 19.9 32.9 13.0 0.75 0.07 4.2 3.1 2.8 3.5 13.7 17.2 13.1
6 35.3 44.8 9.5 0.68 0.11 4.1 2.2 1.7 2.0 9.9 10.5 13.0
7 18.6 44.4 25.8 0.83 0.06 4.2 2.4 2.7 3.1 12.3 17.7 14.0
8 27.8 35.3 7.5 0.71 0.03 4.2 2.4 2.3 2.6 11.5 15.3 10.2
9 24.6 29.3 4.7 0.98 0.05 4.2 3.2 3.4 4.4 15.2 19.7 11.8
Max 35.3 45.0 25.8 0.98 0.11 4.2 3.2 3.4 4.4 15.2 19.7 14.0
Min 18.6 29.3 4.7 0.66 0.03 4.0 2.0 1.7 2.0 9.9 10.5 10.2
Avg. 23.9 37.8 13.9 0.77 0.08 4.1 2.5 2.5 2.9 12.0 15.7 12.4
σ 5.2 5.8 7.4 0.10 0.03 0.1 0.4 0.5 0.7 1.7 3.0 1.2
σ % 21.6 15.5 53.5 13.05 37.28 2.5 16.7 20.3 25.7 14.0 18.9 9.4

Table C.6. Summary of isothermal robust test results of HW 95 (Alma Center, WI) mortar
mixes at 20oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 13.7 20.5 6.8 2.60 0.23 4.1 5.3 11.3 15.0 35.8 25.7 NA
2 14.8 20.5 5.7 2.54 0.22 3.7 4.7 10.3 14.8 33.5 24.9 NA
3 12.2 19.0 6.8 2.48 0.23 4.1 6.5 12.7 14.0 37.3 22.4 NA
4 18.6 23.9 5.3 2.36 0.26 4.2 3.5 6.5 12.6 26.8 23.6 NA
5 11.4 18.5 7.1 2.65 0.26 3.9 7.9 14.6 14.5 40.9 25.6 NA
6 19.4 25.1 5.7 2.21 0.25 3.8 3.0 5.2 10.7 22.7 23.9 NA
7 12.3 19.4 7.1 2.70 0.25 3.5 6.1 13.2 15.3 38.1 26.6 NA
8 18.2 21.6 3.4 2.31 0.25 4.1 3.9 8.2 13.3 29.5 21.9 NA
9 9.8 15.1 5.3 2.59 0.27 4.5 10.2 15.3 13.7 43.7 23.8 NA
Max 19.4 25.1 7.1 2.70 0.27 4.5 10.2 15.3 15.3 43.7 26.6 NA
Min 9.8 15.1 3.4 2.21 0.22 3.5 3.0 5.2 10.7 22.7 21.9 NA
Avg. 14.5 20.4 5.9 2.49 0.25 4.0 5.7 10.8 13.8 34.3 24.3 NA
σ 3.5 3.0 1.2 0.17 0.02 0.3 2.3 3.6 1.4 6.8 1.6 NA
σ% 23.9 14.5 20.2 6.80 6.52 7.2 40.8 32.9 10.3 19.9 6.4 NA

C-3
Table C.7. Summary of isothermal robust test results of HW 95 (Alma Center, WI) mortar
mixes at 30oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 11.8 15.0 3.2 4.62 0.65 3.8 14.5 24.4 9.5 52.1 NA NA
2 12.4 15.8 3.4 4.95 0.74 3.1 11.5 25.1 9.9 49.6 NA NA
3 8.4 12.5 4.1 4.41 0.66 4.8 19.1 21.7 8.8 54.3 NA NA
4 12.5 15.5 3.0 4.64 0.71 3.6 10.4 22.1 9.2 45.2 NA NA
5 7.2 11.9 4.7 4.73 0.77 5.2 22.6 22.7 10.2 60.7 NA NA
6 14.2 14.9 0.7 5.00 1.04 3.4 9.7 20.1 9.4 42.6 NA NA
7 7.9 11.9 4.0 4.83 0.77 4.7 21.5 23.0 9.9 59.1 NA NA
8 11.5 14.4 3.0 4.32 0.60 4.7 14.6 20.2 8.1 47.6 NA NA
9 6.1 10.9 4.7 4.54 0.80 7.9 25.2 19.0 8.7 60.9 NA NA
Max 14.2 15.8 4.7 5.00 1.04 7.9 25.2 25.1 10.2 60.9 NA NA
Min 6.1 10.9 0.7 4.32 0.60 3.1 9.7 19.0 8.1 42.6 NA NA
Avg. 10.2 13.6 3.4 4.67 0.75 4.6 16.6 22.0 9.3 52.5 NA NA
σ 2.8 1.8 1.2 0.23 0.13 1.4 5.7 2.0 0.7 6.8 NA NA
σ% 27.9 13.5 36.3 4.97 17.10 31.5 34.4 9.1 7.4 12.9 NA NA

Table C.8. Summary of isothermal robust test results of HW 95 (Alma Center, WI) mortar
mixes at 40oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 7.2 9.3 2.1 6.49 1.81 7.6 35.8 14.4 9.3 67.1 NA NA
2 9.1 9.6 0.5 7.66 2.25 5.3 34.3 16.1 10.6 66.2 NA NA
3 5.2 9.1 3.9 5.92 1.48 9.4 35.0 13.0 8.1 65.5 NA NA
4 9.1 9.4 0.4 5.45 3.56 5.2 28.3 15.1 10.2 58.9 NA NA
5 4.9 7.9 3.0 5.33 1.54 12.4 37.0 13.1 8.1 70.5 NA NA
6 9.3 9.7 0.4 6.58 4.24 3.9 25.4 15.9 11.5 56.7 NA NA
7 7.2 9.1 1.9 6.97 1.92 7.8 39.5 15.0 9.2 71.6 NA NA
8 9.1 9.5 0.4 5.90 1.77 6.4 30.1 13.4 9.0 58.9 NA NA
9 4.1 7.1 3.0 4.86 0.68 16.3 34.9 12.1 7.1 70.4 NA NA
Max 9.3 9.7 3.9 7.66 4.24 16.3 39.5 16.1 11.5 71.6 NA NA
Min 4.1 7.1 0.4 4.86 0.68 3.9 25.4 12.1 7.1 56.7 NA NA
Avg. 7.2 9.0 1.7 6.13 2.14 8.3 33.4 14.2 9.2 65.1 NA NA
σ 2.1 0.9 1.4 0.88 1.10 3.9 4.5 1.4 1.4 5.6 NA NA
σ% 28.5 9.9 78.6 14.36 51.43 47.7 13.5 9.9 14.9 8.6 NA NA

C-4
Table C.9. Summary of isothermal robust test results of US 63 bypass (Ottumwa, IA)
mortar mixes at 10oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 18.5 25.7 7.2 1.59 0.13 3.8 2.8 5.1 8.6 20.3 25.9 9.9
2 22.4 31.4 8.9 1.63 0.12 4.4 2.2 2.9 5.6 15.0 29.8 12.2
3 14.0 21.0 7.0 1.67 0.12 3.8 3.8 7.3 9.9 24.8 24.2 9.4
4 19.7 29.4 9.7 1.58 0.12 4.5 2.6 4.2 7.5 18.8 25.7 10.6
5 16.3 21.5 5.2 1.75 0.14 3.6 3.9 7.6 10.3 25.4 25.7 10.0
6 20.4 31.3 10.9 1.52 0.11 4.7 2.4 3.1 5.5 15.6 26.6 11.3
7 17.4 26.2 8.8 1.57 0.12 3.9 2.8 4.3 7.8 18.8 28.0 11.4
8 17.3 25.9 8.6 1.58 0.11 4.2 3.5 6.4 9.1 23.2 23.2 9.6
9 14.5 18.6 4.1 1.81 0.16 3.9 5.1 9.2 10.6 28.8 24.1 9.5
Max 22.4 31.4 10.9 1.81 0.16 4.7 5.1 9.2 10.6 28.8 29.8 12.2
Min 14.0 18.6 4.1 1.52 0.11 3.6 2.2 2.9 5.5 15.0 23.2 9.4
Avg. 17.8 25.6 7.8 1.63 0.13 4.1 3.2 5.6 8.3 21.2 25.9 10.4
σ 2.7 4.6 2.2 0.09 0.02 0.4 0.9 2.2 1.9 4.7 2.0 1.0
σ% 15.4 17.8 27.6 5.79 12.07 9.1 28.8 39.5 22.7 22.0 7.9 9.6

Table C.10. Summary of isothermal robust test results of US 63 bypass (Ottumwa, IA)
mortar mixes at 20oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 8.6 13.2 4.7 3.12 0.46 3.9 11.5 17.9 9.1 42.4 16.7 NA
2 12.0 16.9 4.8 3.11 0.52 3.5 6.5 17.5 12.2 39.6 18.0 NA
3 7.1 11.8 4.7 3.22 0.48 4.4 15.1 17.4 8.1 44.9 15.6 NA
4 11.3 16.8 5.5 3.10 0.43 3.8 8.4 17.4 8.8 38.5 17.2 NA
5 10.6 13.2 2.6 3.07 0.48 3.2 10.6 17.3 10.0 41.1 15.7 NA
6 12.9 18.5 5.6 3.06 0.48 4.0 4.3 14.8 12.2 35.4 18.6 NA
7 11.7 14.8 3.2 3.35 0.60 3.2 7.7 19.1 12.9 42.9 18.4 NA
8 8.3 15.8 7.5 3.10 0.42 3.9 11.7 17.4 7.6 40.6 16.1 NA
9 6.3 10.2 3.9 3.52 0.54 5.7 18.8 16.3 8.1 48.8 14.6 NA
Max 12.9 18.5 7.5 3.52 0.60 5.7 18.8 19.1 12.9 48.8 18.6 NA
Min 6.3 10.2 2.6 3.06 0.42 3.2 4.3 14.8 7.6 35.4 14.6 NA
Avg. 9.9 14.6 4.7 3.18 0.49 4.0 10.5 17.2 9.9 41.6 16.8 NA
σ 2.3 2.7 1.4 0.16 0.06 0.8 4.4 1.2 2.0 3.8 1.4 NA
σ% 23.8 18.4 30.7 4.89 11.60 19.4 42.3 6.8 20.6 9.3 8.2 NA

C-5
Table C.11. Summary of isothermal robust test results of US 63 bypass (Ottumwa, IA)
mortar mixes at 30oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 6.9 9.7 2.7 5.44 1.46 5.9 28.2 11.3 7.9 53.3 NA NA
2 8.2 11.2 3.0 5.68 1.62 3.3 24.5 14.7 8.8 51.3 NA NA
3 4.9 7.5 2.7 4.79 1.24 9.6 28.5 10.6 7.2 55.9 NA NA
4 7.4 10.4 3.0 5.65 1.37 4.9 26.0 11.4 8.0 50.3 NA NA
5 6.4 8.1 1.7 5.30 1.66 6.8 30.5 11.4 7.6 56.3 NA NA
6 7.9 11.1 3.2 5.61 1.48 3.7 23.7 13.1 8.6 49.1 NA NA
7 7.7 9.8 2.1 5.88 1.85 3.7 28.4 13.8 8.5 54.3 NA NA
8 5.3 9.5 4.3 5.00 1.05 8.3 27.2 10.3 7.0 52.8 NA NA
9 4.5 6.9 2.4 4.25 1.15 12.3 28.9 10.3 6.9 58.3 NA NA
Max 8.2 11.2 4.3 5.88 1.85 12.3 30.5 14.7 8.8 58.3 NA NA
Min 4.5 6.9 1.7 4.25 1.05 3.3 23.7 10.3 6.9 49.1 NA NA
Avg. 6.6 9.3 2.8 5.29 1.43 6.5 27.3 11.9 7.8 53.5 NA NA
σ 1.4 1.5 0.7 0.52 0.26 3.1 2.2 1.6 0.7 3.0 NA NA
σ% 21.3 16.5 26.6 9.84 18.19 47.4 8.1 13.4 9.2 5.6 NA NA

Table C.12. Summary of isothermal robust test results of US 63 bypass (Ottumwa, IA)
mortar mixes at 40oC
FS-IS Peak Peak
IS, h FS, h ,h rate slope A1-6h A6-12h A12-18h A18-24h A1-24h A24-48h A48-72h
1 4.1 5.8 1.7 9.23 4.27 22.8 24.7 11.3 8.5 67.4 NA NA
2 5.3 7.3 2.0 8.94 3.25 10.9 30.6 13.3 9.8 64.6 NA NA
3 4.1 5.8 1.7 9.18 4.25 23.0 24.4 11.2 8.4 67.1 NA NA
4 5.2 7.2 2.0 8.77 3.19 11.1 29.8 13.0 9.6 63.5 NA NA
5 4.3 5.7 1.4 9.89 4.88 23.1 25.8 11.6 8.6 69.1 NA NA
6 6.9 8.2 1.3 8.34 2.74 5.0 30.5 14.8 10.3 60.6 NA NA
7 5.4 7.0 1.6 9.96 4.50 10.2 34.1 14.2 9.8 68.3 NA NA
8 4.2 6.3 2.1 8.71 3.59 18.4 24.8 11.6 8.7 63.5 NA NA
9 4.0 5.3 1.3 9.82 4.90 25.7 23.5 11.3 8.6 69.1 NA NA
Max 6.9 8.2 2.1 9.96 4.90 25.7 34.1 14.8 10.3 69.1 NA NA
Min 4.0 5.3 1.3 8.34 2.74 5.0 23.5 11.2 8.4 60.6 NA NA
Avg. 4.8 6.5 1.7 9.20 3.95 16.7 27.6 12.5 9.2 65.9 NA NA
σ 1.0 0.9 0.3 0.58 0.79 7.5 3.7 1.4 0.7 3.0 NA NA
σ% 20.0 14.6 18.1 6.29 19.89 44.7 13.5 10.9 7.8 4.5 NA NA

C-6
Table C.13. Summary of robust isothermal test results of US 71 (Atlantic, IA) mixes
5oC- 20oC- 20oC- 30oC- 30oC- 40oC- 40oC-
avg. 5oC-σ avg. σ avg. σ avg. σ
IS, h 20.70 4.60 12.8 3.1 9.8 3.8 6.2 0.8
FS, h 29.40 2.90 19.8 5.7 12.4 2.8 8.6 1.3
FS-IS, h 8.70 1.80 7.0 3.2 2.6 1.9 2.4 0.7
Peak rate 1.25 0.13 2.5 0.2 4.6 0.2 5.1 1.4
Peak slope 0.08 0.01 0.3 0.1 1.1 0.1 2.4 0.8
A1-6h 4.06 0.33 3.7 0.3 4.1 0.9 7.1 3.6
A6-12h 2.72 0.45 5.7 2.9 18.6 5.4 31.6 2.6
A12-18h 3.74 1.23 12.1 3.7 19.9 1.9 10.8 0.8
A18-24h 5.55 1.70 12.5 0.9 7.5 0.7 7.4 0.5
A1-24h 16.06 3.05 33.9 6.3 50.0 5.0 56.8 4.6
A24-48h 26.09 1.56 22.6 2.0 NA NA NA NA
A48-72h 12.54 1.55 NA NA NA NA NA NA

Table C.14. Summary of robust isothermal test results of HW 95 (Alma Center, WI) mixes
5oC- 20oC- 20oC- 30oC- 30oC- 40oC- 40oC-
avg. 5oC-σ avg. σ avg. σ avg. σ
IS, h 23.90 5.20 14.5 3.5 10.2 2.8 7.2 2.1
FS, h 37.80 5.80 20.4 3.0 13.6 1.8 9.0 0.9
FS-IS, h 13.90 7.40 5.9 1.2 3.4 1.2 1.7 1.4
Peak rate 0.77 0.10 2.5 0.2 4.7 0.2 6.1 0.9
Peak slope 0.08 0.03 0.2 0.0 0.8 0.1 2.1 1.1
A1-6h 4.12 0.10 4.0 0.3 4.6 1.4 8.3 3.9
A6-12h 2.51 0.42 5.7 2.3 16.6 5.7 33.4 4.5
A12-18h 2.46 0.50 10.8 3.6 22.0 2.0 14.2 1.4
A18-24h 2.89 0.74 13.8 1.4 9.3 0.7 9.2 1.4
A1-24h 11.98 1.68 34.3 6.8 52.5 6.8 65.1 5.6
A24-48h 15.74 2.97 24.3 1.6 NA NA NA NA
A48-72h 12.41 1.16 NA NA NA NA NA NA

C-7
Table C.15. Summary of robust isothermal test results of US 63 bypass (Ottumwa, IA)
mixes
5oC- 20oC- 20oC- 30oC- 30oC- 40oC- 40oC-
avg. 5oC-σ avg. σ avg. σ avg. σ
IS, h 23.90 5.20 14.5 3.5 10.2 2.8 7.2 2.1
FS, h 37.80 5.80 20.4 3.0 13.6 1.8 9.0 0.9
FS-IS, h 13.90 7.40 5.9 1.2 3.4 1.2 1.7 1.4
Peak rate 0.77 0.10 2.5 0.2 4.7 0.2 6.1 0.9
Peak slope 0.08 0.03 0.2 0.0 0.8 0.1 2.1 1.1
A1-6h 4.12 0.10 4.0 0.3 4.6 1.4 8.3 3.9
A6-12h 2.51 0.42 5.7 2.3 16.6 5.7 33.4 4.5
A12-18h 2.46 0.50 10.8 3.6 22.0 2.0 14.2 1.4
A18-24h 2.89 0.74 13.8 1.4 9.3 0.7 9.2 1.4
A1-24h 11.98 1.68 34.3 6.8 52.5 6.8 65.1 5.6
A24-48h 15.74 2.97 24.3 1.6 NA NA NA NA
A48-72h 12.41 1.16 NA NA NA NA NA NA

C-8
APPENDIX D: CALIBRATION OF THE CALORIMETER

Calibration sample preparation

1. Put 60 grams of epoxy in the plastic cup and wait until the epoxy becomes hard.
2. Put a 50Ω resistor in the middle of the cup and add 120 grams of epoxy.
3. Set the cup still and let the epoxy harden.
4. Connect four calibration cups in series.
5. Connect these two serial sets in parallel.

Calibration setting file

1. Open PicoLog Recorder. If a welcome message is displayed as the following,
select Normal.

2. The PLW Recorder window is displayed

3. Click the New Settings from File dropdown menu, and select. The Recording
window appears.

D-1
4. Select Real time continuous for Recording method. Define Stop as the Action at
end of run and ignore other options, then press OK.
5. The Sampling Rate dialogue box is displayed.
6. Input the Sampling interval and the Maximum number of samples and then click
OK.

7. The Converter details dialogue box is displayed. Select TC08 (serial) for
converter type and COM 1 or the port in use for Port. By clicking on Status,
communication between the calorimeter and the PC will be confirmed. Press OK.

D-2
8. The TC08 Channels dialogue box is displayed. Highlight the first channel to be
defined. Click on Edit.

9. The Edit TC08 Channel dialogue box is displayed. Accept the default name of
Channel 1 in the Name field. Select mV from the dropdown menu for the
Thermocouple type. Do not check the Filter Enable box. From the Edit TC08
Channel dialogue box, click on the Options button.

10. The Parameter options dialogue box is displayed. In the Units box, select mV.
Input the desired numbers for the Number display and Scaling for graphs. Click
OK twice until it goes back to the TC08 Channel dialogue box. Repeat the same
procedure for the remaining channels. After defining all eight channels, click OK
to accept all channels at the same time.

D-3
 11. The display automatically reverts to PLW Recorder. To save these settings for use
later, select Save As from the File dropdown menu. File must be saved with the
extension .pls.
12. The parameters for the calibration are now complete.

Calibration process
1. Turn on the computer and open the software PicoLog Recorder.
2. Click Open from File dropdown menu. The Open file dialogue box is displayed.
Select the setting file created following the above procedures.
3. With the calibration setting file selected, click Open from File dropdown menu.
4. The Create new file dialogue box is displayed. Enter the file name for the
experiment. Use a maximum of eight characters to describe all channels at the
same time. Then press OK. Make sure the file has the extension .plw, which is for
data files.

1. The PLW Recorder dialogue box is displayed, showing Ready to Start along with
the number of data points to be collected and the frequency of collection. The
defined channels are listed below, showing the millivolt values for each channel.

D-4
2. To start recording data, click the red START RECORDING button at the left top
of the PLW Recorder window. A message in the PLW Recorder dialogue box
shows the number of data points collected. The count will continuously update as
data samples are collected.

3. A curve of the collected values for each channel can be displayed by clicking the
Graph button on the right top of the PLW Recorder dialogue box.

4. When the baseline is stable, allow it to be recorded for 5 minutes (UBL before).
5. Turn on the voltage generator.
6. Keep the voltage at a constant value until a steady state signal is displayed on the

D-5
 graph (Usteady). The resistors inside the calibration unit are the same. Therefore,
the rate of heat evolution for each channel is the same.
7. Shut down the voltage generator and keep the test running.
8. Wait until the signal is stable again and record a baseline for 5 to 10 minutes (UBL
after). Then stop the test.
9. Calculate the calibration factor (ε) for each channel according to the following
equations
U BLbefore + U BLafter
U BLmean =
2
U steady state adjust = U steady state − U BL mean

ε = p / U steady state adjust

Where, p is the calculated rate of heat production.

D-6
APPENDIX E: PROPOSED SPECIFICATION FOR MONITORING HEAT
EVOLUTION OF CEMENTITIOUS MATERIALS USING A SIMPLE ISOTHERMAL
CALORIMETRY TECHQUE (VERSION 2)

The following is a test method for monitoring heat evolution of cementitious materials in mortar
or concrete using a simple isothermal calorimetry technique.

E.1 Scope

E.1.1

This document describes the test apparatus, procedure, result analysis, and requirements for use
of a simple isothermal calorimeter to monitor heat evolution of cement-based materials.

E.1.2

The values stated in SI units shall be regarded as the standard.

E.1.3

This standard does not purport to address all of the safety concerns, if any, associated with its
use. It is the responsibility of the user of this standard to establish appropriate safety and health
practices and determine the applicability of regularity limitations prior to use.

E.2 Referenced Documents

E.2.1 ASTM Standards

C305 Practice for Mechanical mixing of Hydraulic Cement Pastes and Mortars of Plastic
Consistency

C403/C 403M Standard Test Method for Time of Setting of Concrete Mixtures by Penetration
Resistance

E-1
E.3 Summary of Test Method

E.3.1

This method monitors the heat evolution process of paste or mortar samples, with and without
admixtures and/or additives, under different curing temperatures. A simple isothermal
calorimeter will be used for the test.

E.3.2

The thermal setting times of the tested materials can be estimated from the calorimetry results as
described in the section of calculations.

E.4 Significance and Use

E.4.1

The heat evolution process of a cement-based material is strongly influenced by the chemical and
physical properties of the cement, supplementary cementitious materials (SCMs), chemical
admixtures, mix proportions, construction procedures, and curing conditions. Therefore,
deviations in the quantities and characteristics of the material constituents as well as effects of
construction conditions can be detected by monitoring the heat evolution of the cementitious
material using a simple calorimeter. Research and practice have demonstrated that a calorimetry
test has a high potential for characterizing cementitious material features, detecting the concrete
incompatibility problems, predicting fresh concrete properties (such as set time), and assessing
hardened concrete performance.

E.5 Apparatus

E.5.1 Mixer

The mixer shall comply with practice ASTM C305.

E.5.2 Paddle, Mixing Bowl

Equipment shall comply with practice ASTM C305.

E.5.3 Scraper

The scraper shall consist of a semi-rigid rubber blade attached to a handle about 150 mm long.
The blade shall be about 75 mm long, 50 mm wide, and tapered to a thin edge about 2 mm thick.

E-2
E.5.4 Supplementary Apparatus

The balances, weights, glass graduates and any other supplementary apparatus used in measuring
and preparing the mortar materials prior to mixing shall conform to the respective requirements
for such apparatus as specified in the method for the particular test for which the mortar is being
prepared

E.5.5 Calorimeter and Acquisition System

The isothermal calorimeter is suitable and calibrated to monitor the heat of hydration of cement
paste and mortar in a reproducible fashion. The calorimeter shall be able to provide a testing
temperature within 0°C –60°C ±0.5°C. It shall have three or more test units to allow three or
more repetitions to be performed at the same time. The variation in the maximum rate of heat
evolution between the repeated samples shall be less than 5%. The data acquisition equipment
shall be capable of performing continuous logging of the measurement results with a time
interval of no more than 60 s.

E.5.6 Environment Chamber

The system shall provide the chamber with a constant temperature in a range of 0°C–60 °C.

E.6 Test Specimens

E.6.1

The test specimens can be paste or mortar. The specimen sizes for paste and mortar are 10 g and
100 g, respectively. A repetition of three samples should be tested for each paste or mortar mix.

E.6.2

The batch size should be sufficient to provide homogeneously mixed samples in the mixer used.

E.7 Procedure

E.7.1

Set the environmental chamber at the desired temperature and let the temperature in the chamber
become stabilized.

E.7.2

Program the calorimeter.

E.7.2.1

Click the stop button in the PLW Recorder window to stop the previous test.

E-3
E.7.2.2

Click the New Data from File dropdown menu in the PLW Recorder window.

E.7.2.3

Enter the name of the new file and press OK.

E.7.3

Prepare the paste or mortar sample according to the ASTM C305 method. Record the mixing
time.

E.7.4

Load the specimen into the calorimeter.

E.7.4.1

Weigh and record the empty mass of the plastic sample cup to be used, or tare the scale to zero
with the empty plastic sample cup on the scale.

E.7.4.2

Place the mixed paste or mortar into the plastic sample cup on the scale.

E.7.4.3

Weigh and record the sample to an accuracy of 0.1 g and cover the sample cup with the lid. The
mass of the specimen shall be noted.

E.7.4.4

Immediately place the plastic sample cup into the calorimeter.

E.7.5

Click the start button in the PLW Recorder window and start measuring the heat evolution rate.

E.8. Calculations

E.8.1 Post-Processing of Data

The evaluation method consists of the following steps:

1. Remove the baseline:

E-4
 U (t ) = U raw − U bl

Here Uraw is the signal from the calorimeter and Ubl is the measured baseline of the
calorimeter.
2. Apply the calibration coefficient ( ) and divide by the mass of cement (mc)
ε ⋅ U (t )
P (t ) =
mc
3. Calculate the results as rate of heat evolution, power (mW) as a function of time
and normalize to a unit mass of total cementitious materials (mW/g). The result is
the average of the test specimens. The maximum value of each specimen shall not
be within 5% of the average value. If it is higher than 5%, this value should be
deleted.

E.8.2 Interpretation of The Results

E.8.2.1 Determine the Area underneath the Heat Evolution Curve

The area underneath the curve represents the heat generated during that time. The areas for 1
hour–6 hours, 6 hours–12 hours, 12 hours–18 hours, and 18 hours––24 hours are calculated. The
first hour is not counted because the system needs a certain time for stabilization.

E.8.2.2 Determine the Setting Times

In this method, the first derivative, d(q)/d(t), of a calorimetry curve is derived from the original
heat evolution test data. The initial set time of the tested mortar is defined as the time when the
first derivative curve reaches its highest value. At this point, the increase in the rate of heat
generation is the fastest. After the initial set time, the first derivative value starts to decrease. The
time when the first derivative drops to zero is defined as the final set of the tested mortar. This
point corresponds to the time when the highest rate of hydration is achieved and after this point
the rate of hydration will be reduced. For some samples, the heat evolution curve is similar to
Figure1b. There are three peaks in the positive sides of the heat revolution curve. The initial set
of the tested mortar is still defined as the time at which the first derivative of the heat evolution
curve reaches its highest value. Unlike Figure1a, the first derivative of the rate of heat evolution
of the mortar with FA starts increasing again before descending to zero. In order to determine the
final set under this situation, line A in Figure 1b is extended to cross with the time-axis. This
intersecting point is defined as the final set time of the mortar containing FA.

E-5
 1.0 0.6

0.8
First Derivative A
0.6
0.4 First Derivative
0.4
Final Set 0.2
Final Set
0.2

d (q )/d (t)
d(q)/d(t)

0.0 0.0
-0.2 Initial Set Initial Set
-0.4 -0.2

-0.6
-0.4
-0.8
-1.0 -0.6
0 6 12 18 24 0 6 12 18 24
Time (hour) Time (hour)

(a) (b)

Figure E.1. Determination of set times from heat evolution curve

E.9 Report

E.9.1

The report shall include the following information:

• Source and identity of all materials tested

• Temperature, date, time and duration of test
• Mix proportions
• Any unusual observations, such as early stiffening
• A plotted rate of heat evolution curve
• Calculated area values and setting times

E.10 Precision and Bias

E.10.1 Precision

The variation caused by the equipment and operators shall be less than 5% for the peak value.

E.10.2 Bias

Error of heat evolution test can come from both the testing and data interpreting process. It
should be recommended that the operator of the heat evolution test should be able to perform the
test in a consistent manner. The time from the mortar/concrete mixing to the time the specimen is

E-6
place into the testing device should be well-controlled and documented. Also, it is recommended
that the original temperature of raw materials before mixing should also be controlled; a
difference of the material temperature and testing temperature within 3oC should be required. In
low testing temperature, due to the larger difference of test temperature and room temperature,
and to the lower rate of heat evolution, a higher level of deviation of heat evolution reading is
commonly observed. In order to better interpret the data, a higher degree of smoothing process
can be applied; however, excessive smoothing process can generate bias.

Bias for this test method cannot be determined since there is no reference standard available for
comparison.

E-7