Accelerated Measurement of Goal

Cement Resistance to Sulfate

Attack
Accelerated test and model to predict the
Chiara F
F. Ferraris sulfate resistance of concrete
Paul Stutzman

NIST, Building and Fire Research Laboratory

Sponsored by PCA

Protocol
Select mixture design Select cement: Wet-Dry or temperature
cycles : Proposed test
“Concrete” Mixture design
“cement”

YES Model NO
available
complete
Saturation level
Partial ¾ Partially immersed
Analysis of cement:
Prepare small specimens
Expose them to sulfate
specimen under RH, T
XRD/PSD/other
Diffusion
Sorption controlled RH and
Expansion temperature Paraffin oil
measurementt
Transport
properties based
Cycles Cement
microstructure ¾ Dimension changes
Models based Models
¾ Spalling measurement
Determine concrete Determine cement Salt solution
susceptibility to resistance to sulfate None of the surfaces of the
sulfate ingress attack specimen are protected

Predict service life of structure

Phase diagram Deterioration

Onset Deterioration [days]

140
120
100
88 control
80
89 FA-C
60 •Low RH Î higher deterioration
90 SF
40 •Temp >32 °C Î no deterioration
20 257 d
0
30%, 25C 80%, 25C 80%, 40C
Flatt, J. Cryst. Growth
(2002) T
Treatment
t t
88, 30%
Width deterioration [mm

40
88, 80%
35
30 89, 30%
25
89, 80%
20
15 90, 30%
• Damage done by Mirabilite precipitation 10 90, 80%
Í No damage when temperature stays above 32.4 °C 5
0
• at 20 °C, stresses of 19 MPa according to calculations 0 100 200 300
Time [days]

1
Conditions: 25 °C, RH 30% Conditions: 25 °C, RH 80%

After 40 °C, RH 80%

Conditions: 40 °C, RH 80% placed 25 °C, RH 30%

Control FA-C SF

Protocol
Test and study criteria
Select mixture design Select cement
Mixture design

YES Model NO
applicable
¾ Deterioration Test to ASTM complete
Saturation level
Partial

ƒ Partial immersion Analysis of cement:

Prepare small specimens
Expose them to sulfate
Sorption XRD/PSD/other
ƒ Controlled temperature and RH Diffusion

ƒ Measurement of deterioration: dimensions

Expansion
dimensions, scaling measurementt
Models: Cycles Models
¾ Prediction Test (need further development) • NIST-CONCLIFE
• 4SIGHT
• Mobasher-Tixier
ƒ Porosity and pore size distribution
ƒ Tensile strength
Determine concrete Determine cement
ƒ Surface “strength”: abrasion? Rebound hammer? susceptibility of
sulfate ingress
resistance to sulfate
attack
ƒ Sorption
Predict service life of structure

2
 PCA 174, 64d, outer paste, sulfur distribution
- highly-leached outer zone: approximate
high degree of hydration, line of
decalcified C-S-H, no CH or cracking
ettringite
- gypsum replacement of
calcium hydroxide

Baar Surface
- gypsum-filled fractures.
- no ettringite in outer portion
- X-ray imaging of sulfur shows
progressive migration of Sulfur Distribution
500 μm gypsum-rich zone

Gap after pin lift

about 0.5 mm
PIN
10 mm

Small Specimens mold

Schematic of Deterioration

10 mm side
40 mm long

A
Screws holding pin in place

Small samples - NIST

Large and C1012 – mini
0.7 MA-125A= Type I
MA-125B= Type II
0.6
MA-125C=Type V
3.0
control
C1012 samples

small bars
SF
0.5
2.5 GGBFS-80
Expansion [%]
Expansion [%]

GGBFS-100 0.4
2.0
0.3

Collaboration with
1.5
Start [days]
0.2
1.0 small standard
0.5 Type I/II 19 90 0.1
Doug Hooton
0.0 SF >80 >600 0
0 50 100 150 200 0 50 100 150 200 250
GGFS80 37 139
Time [days]
GGFS100 37 139
Time [days]
1.6
C1012 data by Doug Hooton
0.7
0 7
Type I/II 1.4 TypeI I
0.6 Type

3-5 times faster !

3.0 SF
GGFS80 1.2 TypeIIII
Type
2.5 GGFS100 0.5
Expansion [%]
[%]
Expansion [%]

1.0 Type
TypeVV
2.0
Expansion

0.4
1.5 0.8
0.3
1.0 0.6
0.5 0.2
0.4
0.0 0.1
0.2
-0.5
0.0
0 50 100 150 200 0.0
0 50 100 150 200 250
0 100 200 300 400 500 600 700 800
time [days] small samples Time [days]
Time [days]

3
 Protocol
Small sample future tests
Select mixture design Select cement
Mixture design

YES Model NO
applicable
complete Partial
Saturation level
¾Establish correlation with ASTM C1012 Analysis of cement:
Prepare small specimens
Expose them to sulfate

ƒ Need more cements with C1012 data Diffusion

Sorption XRD/PSD/other

ƒ Field correlation Expansion

measurementt
Models: Cycles Models

¾Procedure in discussion at ASTM • NIST-CONCLIFE

• 4SIGHT
• Mobasher-Tixier

ƒ Round-robin to validate the procedure: On

going Determine concrete Determine cement
susceptibility of resistance to sulfate
ƒ Ballot sulfate ingress attack

Predict service life of structure

Acknowledgements
¾ Max Peltz Thank you
¾John Winpigler
¾Dr Kenneth Snyder
¾Dr.
¾Dr. Paul Tennis
¾PCA for funding
Questions?