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Corrosion of Post-Tensioned Tendons with Deficient Grout.Part 3: Segregated

Grout with Elevated Sulfate and Vestigial Chloride Content

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DOI: 10.5006/3097

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ENGINEERING SECTION

Corrosion of Post-Tensioned Tendons with

Deficient Grout, Part 3: Segregated Grout
with Elevated Sulfate and Vestigial
Chloride Content

S. Permeh,‡,* K.K. Krishna Vigneshwaran,* K. Lau,* and I. Lasa**

Severe corrosion of post-tensioned (PT) tendons with pre-packaged thixotropic grout was documented in Florida bridges after less than
8 years of service. In those bridges, corrosion of steel tendon components was associated with deficient grout characterized by high moisture
content, high sulfate levels, low chloride levels, and no indication of carbonation. Earlier research described in Parts 1 and 2 of this series of
papers had emphasis on the role of sulfate ions in corrosion. However, at the time of observed corrosion of the bridge tendons in deficient
grout, there were separate cases of bridges with similar pre-packaged grout materials but containing significant chloride ion contamination
that exceeded typical acceptance limits. As a response to the potential risk to the bridge inventory, research was conducted to assess the risk
associated with elevated chloride levels. Recommendations were made, but the proposed limits did not directly consider the effect of grout
deficiencies such as that observed in the tendon failures in Florida. Therefore, there was interest to verify that the corrosion risk assessment of
PT tendons by grout chloride concentration is adequate for adverse grout conditions such as due to segregation. In continuation of this
series of papers on corrosion of post-tension strand in physically and chemically deficient grout, the work presented here sought to verify
the role of elevated free sulfate ion concentrations in segregated grout containing low-level chlorides. Small and large scale laboratory
specimens with geometries allowing for mix water volume displacement produced deficient grout. Physical and chemical deficiencies in
segregated grout reduced the extent of chloride binding. Corrosion activity developed in grout with elevated sulfate concentrations.
However, there were synergistic effects to reduce corrosion resistance for grouts with the combined presence of sulfate and chloride ions.
It was shown that corrosion currents increased for steel in deficient grouts with elevated sulfate levels with the presence of low-level chloride
ions (below conventional chloride threshold values). It was therefore evident that the assessment of corrosion susceptibility in deficient grout
by chloride values alone is insufficient as sulfate ion presence and grout characteristics are also important.

KEY WORDS: chloride, corrosion, grout segregation, post-tensioned tendons, sulfate

INTRODUCTION
S evere corrosion of post-tensioned (PT) tendons with pre-
packaged thixotropic grout was documented in Florida bridges
after less than 8 y of service.1-5 In those bridges, corrosion of
steel tendon components was associated with deficient grout
characterized by high moisture content, high sulfate levels, low
chloride levels, and no indication of carbonation.1
Results of electrochemical testing of steel in alkaline
sodium sulfate solution described in Part 16 of this series of
papers indicated that at pH 12.6, early presence of sulfate ions
(>4,000 ppm sodium sulfate) in solution could be aggressive by
impairing initial passive film development. The instability of the
developing passive film in sulfate alkaline solutions resulted in
formation of pits on the steel surface.6 However, in prepas-
sivated conditions, later incremental additions of sulfates (even
as high as 65,000 ppm sodium sulfate) did not depassivate
steel. Testing described in Part 27 of this series of papers
incorporated grout products mixed past designated expiration
dates and with extra mix water (15% excess of recommended
levels) to promote grout deficiency. Testing indicated that
sulfate ions accumulated in the segregated grout from the
original grout material and not necessarily from external
sources. In the modified inclined tube (MIT) tests, enhanced steel
corrosion activity occurred in deficient grout that had en-
hanced sulfate ion content (typically exceeding 0.1% of the grout
mass), high moisture content (<70%), and 11 < pH < 13.7
At the time of observed corrosion of the bridge tendons
in deficient grout, there were separate cases of bridges with
similar pre-packaged grout materials but containing significant
chloride ion contamination.8-9 The discovery of elevated chlor-
ides in grout from a construction project in Texas in 2010 led
to research on chloride thresholds in tendons. The chloride
content in early testing was estimated to be as high as 5 wt%
by cement,10 and other authors reported chloride ion concen-
trations as high as 0.5 wt% by cement.8 Nevertheless, these
values exceeded typical acceptance limits.11-14 Chloride limits for
prestressed concrete provided by American Concrete

Submitted for publication: November 8, 2018. Revised and accepted: February 23, 2019. Preprint available online: February 23, 2019, https://doi.org/10.5006/3097.
‡
Corresponding author. E-mail: samanbar.permeh1@fiu.edu.
* Florida International University, Dept. of Civil and Environmental Engineering, 10555 W. Flagler St., Miami, FL 33174.
** State Materials Office, Florida Department of Transportation, 5007 N.E. 39th Avenue, Gainesville, FL 32609.

ISSN 0010-9312 (print), 1938-159X (online) © 2019 NACE International.

848 JULY 2019 • Vol. 75 • Issue 7 Reproduction or redistribution of this article in any form CORROSIONJOURNAL.ORG
is prohibited without express permission from the publisher.

Table 1. Grout Mix Condition for MIT Samples(A)
Sample Condition Mix Water Grout Weight (lb)
Base 88.4 lb tap water 297.1
(Gainesville, FL)
Sulfate 1 88.5 lb tap water 296.1
(Gainesville, FL)
Sulfate 2 86.5 lb tap water 289.4
(Gainesville, FL)
Sulfate 3 107.0 lb tap water 296.7
(Gainesville, FL)
Chloride 1 90.3 lb tap water 301.9
(Gainesville, FL)
2.8 g NaCl/L H2O
Chloride 2 89.9 lb tap water 300.5
(Gainesville, FL)
7.0 g NaCl/L H2O
(A)
Each batch mixed with high shear colloidal mixer per manufacturer specification.
Institute (ACI) are either 0.06 wt% water-soluble chloride by
cement or 0.08 wt% acid-soluble chloride by cement.11-12
Current Post-Tensioning Institute (PTI) guidelines allow a maxi-
mum chloride ion content of 0.08 wt% by cement content of
0.03% by mixed grout.14 An investigation by Lee and Zielske
examined chloride ion threshold concentrations for PT ten-
dons.12,15 In that research, steel strand was cast in mockup
tendons using a pre-packaged grout product with enhanced
concentrations of chloride ions ranging from 0.08 wt% to 2 wt%
by cement. Results from testing showed corrosion develop-
ment above 0.4 wt% chloride ion concentration by cement for
strand embedded in normally hydrated grout and indicated
chloride ion threshold limits as low as 0.2%.8 It is noted that the
proposed limits did not directly consider the effect of grout
deficiencies such as that observed in the tendon failures in
Florida.
Grout segregation can create conditions where a general
assessment of chloride content alone may not well assess cor-
rosion risk. For example, segregation can cause an increase in
the local concentration of ionic species. In the previous work,1,7
it was observed that segregated grout can have higher con-
centrations of alkalis, sulfates, and in some instances chloride
ions.(1) Thus, insufficient sampling of deficient grout following
the proposed chloride limits could give a false negative error.
Even with low-level chlorides (within traditional threshold
values), the presence of elevated sulfate ion concentrations may
have synergistic effects with the chloride ions to reduce
corrosion resistance.16-21 For example, Dehwah, et al.,20 indi-
cated corrosion rates in reinforced concrete test samples up
to 2.2 times greater in exposure solutions containing both
chlorides and sulfates than in comparative samples exposed
to solutions with only chlorides. In that testing, corrosion initiation
times were similar for samples in both exposure solutions.
Also, Holden and Page16 indicated that the presence of sulfate
ions can reduce the chloride binding capacity of cement due to
the effects of initial reaction of sulfate ions with C3A. The re-
duction of binding capacity would thus allow higher concen-
trations of free chloride ions in the cement pore water solution.
Testing presented here was to assess the role of phys-
ically and chemically deficient PT grout on strand corrosion and
(1)
Observed elevated total chloride concentrations in part due to oversampling
of dried deficient grout.
CORROSIONJOURNAL.ORG
ENGINEERING SECTION
Admixed Sodium Sulfate Admixed Chloride
Concentration Concentration
0 0
2,000 ppm 0
20,000 ppm 0
150,000 ppm 0
0 ∼0.08 wt% cement
0 ∼0.2 wt% cement
to verify the role of low-level chlorides in segregated grout
containing elevated sulfate ion concentrations. In addition, the
combined effect of chloride ion and elevated sulfate ion
concentrations and the determination of what concentrations
can be accepted as conservative threshold values for these
cases with segregated grout will be addressed.
EXPERIMENTAL PROCEDURES
2.1 | Modified Incline Tube Test and Inverted Tee Test
The MIT test, defined by Hamilton, et al.,22 was used for
sample preparation. Placement of steel corrosion probes along the
length of the tube allowed assessment of steel corrosion with
varying degrees of grout deficiency due to segregation associated
with vertical elevation deviation. Fifteen-foot (4.57 m) long MIT
samples were cast with expired grout materials with 15% excess
mix water and inclined at 30° from the horizon. Two 7-wire
unstressed steel strands were embedded within the duct. Further
details on the MIT test were elaborated in Part 2 of this series of
papers.7 The corrosion probes were placed at five points along the
length of the tendons. Each probe contained a three-electrode
arrangement for conducting electrochemical measurements.
An activated titanium rod (periodically calibrated with a copper/
copper-sulfate reference electrode [CSE]) and an embedded
activated titanium mesh placed along the length of the tendon
were used as the reference and counter electrode, respectively.
Duplicate samples were made for each testing condition. Grout
test conditions were made, as listed in Table 1.
The inverted tee test (INT) was developed as a simpler
test to supplement the larger MIT test. The geometry of the
inverted polyvinyl chloride (PVC) tees facilitated volume
displacement of deficient grout material to the tee header,
where low density bulk material and water from the base
would accumulate in the smaller stem portion of the PVC tee.
This allowed discrete testing and sampling of the dissimilar
grout materials. The test samples utilized grout that was pre-
exposed for 1 month in high-humidity conditions and mixed
with 20% excess water with varying sodium sulfate and sodium
chloride additions. The control set of the samples were cast
with as-received grout following the manufacturer recom-
mended mix water content but contained different sodium
sulfate concentrations (0 ppm, 2,000 ppm, and 20,000 ppm).
JULY 2019 • Vol. 75 • Issue 7 849
ENGINEERING SECTION

Table 2. Grout Mix Condition for INT Samples(A)

Sodium Sulfate Chloride Amount
Test Case Grout Condition Mix Water Grout Weight (lb) Amount (ppm) (% by Cement)
Control Base As-Rec’d 0.64 L tap water (Miami, FL) 5.2 0 0
Sulfate 1 As-Rec’d 0.64 L tap water (Miami, FL): 5.2 2,000 0
Sulfate 2 As-Rec’d 0.64 L tap water (Miami, FL): 5.2 20,000 0
Test Base Pre-Exposed 0.77 L tap water (Miami, FL) 5.2 0 0
Sulfate 1 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 2,000 0
Sulfate 2 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 20,000 0
Sulfate 3 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 100,000 0
Chloride 1 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 0 0.08
2.083 g NaCl/L H2O
Chloride 2 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 0 0.2
5.206 g NaCl/L H2O
Combined 1 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 2,000 0.08
2.083 g NaCl/L H2O
Combined 2 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 20,000 0.08
2.083 g NaCl/L H2O
Combined 3 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 100,000 0.08
2.083 g NaCl/L H2O
Combined 4 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 2,000 0.2
5.206 g NaCl/L H2O
Combined 5 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 20,000 0.2
5.206 g NaCl/L H2O
Combined 6 Pre-Exposed 0.77 L tap water (Miami, FL): 5.2 100,000 0.2
5.206 g NaCl/L H2O
(A)
Each batch mixed for 3 min at 600 rpm.

Table 2 lists the test cases and grout mix conditions. The
samples contained embedded high-strength carbon steel wire
probes within the tee header as well as within the tee body. An
embedded activated titanium wire was used as a reference
electrode during polarization tests. An embedded stainless
steel rod was used as the counter electrode. Duplicate samples
were made and tested for each test case. Sample setup and
dimensions are shown in Figure 1.
2.2 | Corrosion Measurements
The corrosion potential (Ecorr) was measured with a CSE
introduced through a side access port. Corrosion current
densities (icorr) of the embedded steel probes were resolved by
determination of the polarization resistance measured by linear
polarization resistance (LPR) method, following Equation (1):
B
icorr = (1)
Rp × A
where the Stern-Geary coefficient (B) was assumed to be 26 mV for
active corrosion conditions and A is the area of the steel probe
exposed to the grout. LPR measurements were made with polar-
ization from the open-circuit condition to −25 mVOCP at a scan
rate of 0.05 mV/s. The resolved apparent Rp was corrected for
3 cm

∅ 5 cm

Carbon steel (WE)

∅ 0.5 cm
7 cm

Stainless steel (CE)

∅ 0.6 cm OCP port
ATR (RE) ∅ 1.27 cm
∅ 0.32 cm

Carbon steel (WE) 13.6 cm

∅ 0.5 cm

FIGURE 1. INT test specimen.

850 JULY 2019 • Vol. 75 • Issue 7 CORROSIONJOURNAL.ORG


voltage drop where the solution resistance RS was measured
following similar three-electrode setup but measured with a soil
resistivity meter.
2.3 | Deficient Grout and Steel Characterization
After electrochemical testing, characterization of the
grout materials included determination of moisture content,
sulfate and chloride content, and leachate pH. Petrography
was done in order to differentiate properties of the deficient
grout. Samples were collected from the tee header and body
for INT specimens and from the upper elevation (∼0.1 m from top)
and lower elevation (∼2 m from top) of the tendons for MIT
tendons.
Moisture content was measured by gravimetric methods
as described in ASTM C566-13.23 An ex situ leaching method
was adopted to obtain grout leachate for chemical and pH
analysis.24 The procedure included drying the powder samples
at 55°C for 24 h and combining 5 g of the dried powder with
1:10 leaching volume at 66°C for 15 h to 18 h. Grout leachate
pH was measured with a pH glass electrode. Sulfate and free
chloride ion analysis was made by ion chromatography. The total
chloride ion concentration was measured following Florida
Method 5-516.25 Steel wires embedded in the deficient/hard
grout were visually inspected at the end of the test. Further
investigation was performed on the cases with corroded wire,
including scanning electron microscopy (SEM) and energy
dispersive x-ray spectroscopy (EDS) analysis.
RESULTS AND DISCUSSION
3.1 | Deficient Grout Characteristics
Deficient grout can be characterized by its physical and
chemical properties. As described earlier and reported else-
where,1 deficient grout from bridge tendons had character-
istics of a porous matrix of segregated grout components
including filler calcite, silica fume, and cement. In laboratory
INT and MIT testing, deficient grout only developed when the
grout was subjected to adverse mixing conditions. Figure 2
shows representative deficient grout from field and laboratory
testing. In those conditions, grout segregation developed.
There the deficient grout only accumulated in the tee header of
INT specimens and at higher elevation (<0.1 m length from
sample top) for MIT test largely due to water volume displace-
ment. Figure 3 shows petrographic micrographs of deficient
and hardened grout from field, INT, and MIT specimens where
grout segregation characteristics were evident. Higher water-
to-cement ratio and high pore content were found for the defi-
cient grout and typically had concentrated agglomerations of
(a)
FIGURE 2. Photos of deficient grout. (a) Field, (b) INT, and (c) MIT.
CORROSIONJOURNAL.ORG
ENGINEERING SECTION
silica fume. The constituency of the deficient grout, as will be
discussed in the following, can affect the material chemistry
and propensity for corrosion of embedded steel elements. Some
level of physical grout segregation was observed (as indicated
by petrographic analysis) in laboratory-cast specimens but the
level of deficiency did not manifest as greatly as observed in
the field. Nevertheless, as discussed in the following, the mois-
ture content and grout leachate pH (Figures 4 and 5) for INT
and MIT test specimens were general indicators differentiating
the deficient and hardened grout.
Figure 4 shows the moisture content for INT and MIT
testing, as well as collected data from Florida PT bridges placed
for comparison. The data show the minimum, maximum, and
average value for each test condition. Laboratory control INT
specimens (grout mixed per recommendation) did not show
any indication of accrued moisture content, and moisture levels
were below 15% within the tee body and tee header. In
comparison, moisture accrued in the tee header (20% to 60%) for
the INT base, sulfate addition, chloride addition, and combined
cases where adverse mixing condition were used, whereas
moisture levels were below 20% in the tee body of the same
samples. MIT testing showed similar trends. The results from INT
and MIT testing were consistent with moisture levels in defi-
cient and hardened grout obtained from field samples, and
consistent with the physical grout attributes observed by
petrography.
Individual moisture data points for laboratory INT and MIT
tests were graphed together as cumulative distribution functions
for the various test conditions as shown in Figure 6. Com-
parative field data were plotted as well. The laboratory control
grout, all grouts in the INT tee body and MIT low elevations, and
hardened grout from the field had moisture content less than
20%. In comparison, laboratory grouts with adverse mix
conditions that separated in the INT tee header, MIT high
elevations, and field deficient grouts had significant sample
populations with moisture content greater than 20% and were as
high as 68% in lab conditions and 80% in the field. More than
50% to 70% of the deficient grout samples either in field or
laboratory had moisture content greater than 20%. From the
collective data in Figure 6, substantial grout segregation can
be identified with moisture levels greater than 20%.
Grout segregation can consequently affect the pore
water pH. The high moisture levels in segregated grout would
allow leaching of hydroxyls from the hydrated cement material
thus providing a high pH bulk solution.26 If atmospheric carbon
dioxide were to be present, carbonation of that bulk solution
may occur.27 Also, the severe segregation of the test grout
material allowed aggregation of admixed silica fume that
can reduce the pH due to consumption of hydroxyl ions.28
(b) (c)
JULY 2019 • Vol. 75 • Issue 7 851
ENGINEERING SECTION

(a) (b)

0.25 mm

100 μm

(c) (d)

25 μm

(e) (f)
FIGURE 3. Petrographic micrographs of deficient and hardened grout. (a, b) Field. (c, d) INT. (e, f) MIT. Left: deficient grout. Right: hardened grout.

100 13.5
90 13
80
Moisture Content (%)

12.5
70
12
60
50 11.5
pH

40 11
30
10.5
20
10
10
0 9.5
Sulfate

Chloride
Base

Comb.

Base

Sulfate

Chloride

Base

Sulfate

Chloride

Comb.

Base

Sulfate

Chloride
Comb.
Base

Sulfate

Base

Base

Comb.

Base
Chloride

Sulfate

Chloride

Sulfate

Chloride

Sulfate

Chloride
Control

Control

Control

Control

Test Test Test Test Test Test Test Test

INT¹ MIT³ Field INT² MIT4 Field INT¹ MIT³ Field INT² MIT4 Field

Deficient (Top) Hardened (Bottom) Deficient (Top) Hardened (Bottom)

FIGURE 4. Moisture content for field and laboratory test. 1: Tee header. FIGURE 5. Grout leachate pH for field and laboratory test. 1: Tee header.
2: Tee body. 3: <0.1 m length from top. 4: >0.1 m length from top. 2: Tee body. 3: <0.1 m length from top. 4: >0.1 m length from top.

852 JULY 2019 • Vol. 75 • Issue 7 CORROSIONJOURNAL.ORG

 ENGINEERING SECTION

1×100

Control
Base:
1 Na2SO4: 2,000 ppm–20,000 ppm

Control mix
1×10–1
0.9 Base:
Na2SO4: 2,000 ppm–150,000 ppm
NaCl: 0.08 wt% cement
0.8 1×10–2 Cl– 0.2 wt% cement

Test
Defficient grout
t

Sulfate Concentration (gSO2–/ggrout)

ed grou
Cumulative Fraction

Comb. Na2SO4 and NaCl:

Cl– 0.08 wt% cement:
0.7 Cl– 0.2 wt% cement:
Controll
1×10–3 Field
Harden

0.6

4
0.5 1×10–4 se
Ba
st
Te
0.4 1×10–5 ld
0.3 1×10–3 Fie
Base:  Control

Sulfate Concentration
–6
Na2SO4 addition:  1×10
0.2 Test

(gSO2– /ggrout)
NaCl addition: 
Comb. Na2SO4 and NaCl addition: 
0.1 1×10–7

4
Field
0
0 20 40 60 80 100 1×10–8
1×10–4
Moisture Content (%) 9 10 11 12 13
Moisture Content (%)
14

1×10–9
FIGURE 6. Moisture content in deficient grout for field and laboratory 1 10 100
test. Dataset includes INT, MIT, and field testing. 20% moisture Moisture Content (%)
content shown as reference. (a)
1×100

Control
Base:
Na2SO4: 2,000 ppm–20,000 ppm
Figure 5 shows the range of pH for grout leachate from the 1×10–1 Base:

Total Cl Concentration (gCl–/ggrout)

laboratory-cast specimens and field samples. The leaching Na2SO4:
NaCl:
2,000 ppm–150,000 ppm
0.08 wt% cement
method for the laboratory samples followed a protocol with an 1×10–2 Cl– 0.2 wt% cement

Test
Comb. Na2SO4 and NaCl:
–
Cl 0.08 wt% cement:
initial dilution ratio of 1:10. The leachate pH was found to be in Cl– 0.2 wt% cement:

range of 10 to 13 for the deficient grout, whereas the hardened 1×10–3 Field
Control
grout had consistently maintained alkaline pH > 12.5. As will be
1×10–4 Field
discussed later, the measured pH between 9.5 and 11.5 for Test Base
certain test cases coincided with the presence of steel corrosion 1×10–5
where the sampled grout contained large portions of corrosion 1×10–3
Total Cl Concentration
Control
products. The lower pH likely developed after corrosion initiation, 1×10 –6
(gCl – /ggrout)

but the conditions described above may not necessarily be

discounted. 1×10–7
Sulfate and chloride ions concentration can be locally
increased by transport mechanisms including diffusion, capillary 1×10–8
1×10–4
suction, and permeation29 by grout segregation to levels that 9 10 11 12
Moisture Content (%)
13 14

1×10–9
can aggravate corrosion conditions. Other chemical changes in 1 10 100
the grout chemistry due to segregation can further heighten Moisture Content (%)
local concentration of ionic species. Figure 7 shows free sulfate (b)
ion, total chloride ion, and free chloride ion concentrations by 1×105
moisture content for all laboratory and field samples. In the figure,
Control

Base:
Na2SO4: 2,000 ppm–20,000 ppm
4
trends in ion accumulation by the level of moisture of the 1×10 Base:
Na2SO4: 2,000 ppm–150,000 ppm
Free Chloride Concentration (ppm)

tested grout are delineated. For the control case that only formed NaCl: 0.08 wt% cement
1×103 Cl– 0.2 wt% cement
Test

hardened grout, each tested sample (regardless of sulfate Comb. Na2SO4 and NaCl:
Cl– 0.08 wt% cement:
additions) had relatively low moisture content (<20%) and rela- –
Cl 0.2 wt% cement:
1×102 Field
tively low ion concentrations (consistent with the relatively
well-hydrated condition), as shown for all data points encom- 1×10 1
t Ba
se Control
Tes
passed in the dashed-lined box. The highest free sulfate ion, Fie
ld
free chloride ion, and total chloride ion concentration in the 1×100
1×102
control (as-received) grout was 0.00042 gsulfate/gpowder, Control
Concentration (ppm)

104 ppm, and 0.00018 gchloride/gpowder, respectively. Dashed lines 1×10–1

Free Chloride

show the trendline for the test base case (except for the salt
1×10–2
addition subcases) and field data. The highest free sulfate ion,
free chloride ion, and total chloride ion concentrations in the 1×10–3
test base case were 0.024 gsulfate/gpowder, 158 ppm, and 1×101
9 10 11 12 13 14
0.00026 gchloride/gpowder, respectively. 1×10–4 Moisture Content (%)

The field data for sulfates and chlorides were overall
lower than from the laboratory testing. The leaching method to
extract sulfate and chloride ions for the field samples yielded
lower concentrations; however, other lab testing described
elsewhere indicated proportional results with the modified
procedures used here.1 Increase in sulfate ion and chloride ion
concentration was apparent in grouts with greater levels of
deficiency quantified by moisture content. The high moisture
1 10 100
Moisture Content (%)
(c)
FIGURE 7. Sulfate and chloride ions concentration by grout defficency.
Dataset includes INT, MIT, and field testing. (a) Sulfate ion, (b) total chloride
ion, and (c) free chloride ion. Dashes show trends for control, test base,
and field grout samples. Gray fields show general trends with respect to
moisture content for test samples with admixed chloride and sulfate.

CORROSIONJOURNAL.ORG JULY 2019 • Vol. 75 • Issue 7 853

ENGINEERING SECTION
levels—in the porous matrix with low cement content and silica
fume aggregation and general indication of lower pH (as sug-
gested earlier)—would have negative effects, heightening the
increase of ion concentration in the segregated grout pore
water. Higher moisture levels would allow for leaching, and
low cement content would not provide cement hydrates to
accommodate ion binding.29 Increase of local of free chloride
ion concentration due to the effects of grout segregation
and changes in grout chemistry in the deficient grout can
be considered of particular interest due to the aggressiveness
of the ions to depassivate steel.13 Figure 8 shows the
cumulative distribution of free chloride ions for each test
condition with various levels of admixed sodium sulfate and
sodium chloride. In contrast, the total chloride concentrations
showed uniform levels regardless of the level of grout seg-
regation (Figure 7[b]).
Free chloride concentrations were higher in deficient
grout in part due to the ionic transport of chloride ions, but bound
chloride concentrations should be relatively lower in the de-
ficient grout than hardened grout due to the lower cement
content in the former. The gray fields in Figure 7 encompass
data for the test cases with salt addition and show similar trends
as the test base and field cases. It was evident that chloride ion
concentrations (developed from vestigial chloride levels from the
pre-packaged grout) were low in the well-hardened grout in the
laboratory control specimens where free chlorides levels were
typically less than 50 ppm, although the data in Figure 8
indicated modest increase in free chloride concentrations in
hardened grout when admixed with sulfates. Approximately
40% of the control test samples admixed with sulfates had
chloride levels greater than the upper free chloride limit in the
control hardened grout mixes. Similar trends were observed for
the test base and sulfate addition cases where deficient grout
developed. With the development of deficient grout, chloride
levels were further elevated (up to 200 ppm in the test base
case and 400 ppm with the addition of sulfates). Even though
some enhancement in free chloride concentrations was ob-
served with the addition of sulfates, the free chloride
1
Control
Base:
Na2SO4: 2,000 ppm–20,000 ppm + Control
0.9 Base:
Na2SO4: 2,000 ppm
20,000 ppm
Test
0.8 NaCl:
100,000 ppm–150,000 ppm
0.08 wt% cement
Cl– 0.2 wt% cement
Comb. Na2SO4 and NaCl:
0.7
Cumulative Fraction
Cl– 0.08 wt% cement:
Cl– 0.2 wt% cement:
0.6
0.5
0.4
0.3
0.2
–1 add
ition
Cl
0.1
SO42– addition
0 discussion.
1 10 100
Free Chloride Concentration (ppm)
FIGURE 8. Free chloride concentration in grout with admixed NaSO2− 4
and NaCl. Gray vertical lines show upper free chloride limit in control
hardened grout mixes at 50 ppm and upper free chloride limit for
segregated grout sans external chloride contaminants at 420 ppm.
854 JULY 2019 • Vol. 75 • Issue 7
concentrations were not commensurate to the level of sulfate
additions. An upper free chloride limit for segregated grout
without external chloride contaminants of 420 ppm was ob-
served based on the results from the test base case and with as
much as 150,000 ppm admixed sodium sulfate. As expected,
higher free chloride concentrations were measured for test
conditions where elevated sodium chloride concentrations
(<0.2 wt% cement) were admixed.
Test cases with combined chloride and sulfate ions
generally only showed modest elevation of free chloride ion
concentrations compared to the admixed chloride cases.
However, the effect of grout segregation was readily apparent.
Combined admixed sulfate/chloride grout mixes in hardened
grout had free chloride concentrations in the range of ∼100 ppm
to 420 ppm, but samples with deficient grout here had ac-
cumulation of chlorides greater than 420 ppm and as high as
∼2,000 ppm regardless of the added chloride levels, reflective
of the higher water-to-cement levels in the deficient grout.
Parsing of the data by grout chemical conditions allowed
for evaluation of the effects of sulfates and chlorides. The graphs
in the Appendix and in later sections are grouped in part by
free chloride levels delineated by the by free chloride levels
described above.
3.2 | Chloride Binding
The chloride concentration measured for the laboratory-
cast grouts with various levels of grout deficiencies is related to
the extent of chloride binding to hydrated cement compo-
nents. Test results showed that the total chloride content was
generally uniform regardless of the extent of grout deficiency,
but free chloride contents were higher for deficient grout. This
would indicate that there is lower proclivity for chloride binding
in deficient grout. The total chloride content and free chloride, as
discussed earlier, was presented as g−Cl =g dry grout and ppm (Cl−
per dry grout mass), respectively, but was converted to
kg−Cl =mgrout 3 by assuming a density of 1,842 kg/m3. This factor
only scales the chloride concentrations without affecting the
following discussion. The bound chloride concentration (CB)
was calculated as the difference between the total chloride
content (CT) and the free chloride content (CF). There were
Base some data outliers where the free chloride content exceeded the
total chloride content due to localized variation in sampling of
the deficient grout. Both Langmuir and Freundlich adsorption
isotherms were considered to identify the relationship be-
tween CB and CF, as shown in Figure 9.30 The Langmuir and
Freundlich isotherms are described by Equations (2) and (3),
respectively:
αCF
CB = (2)
ð1 þ βCF Þ
CB = αCβF (3)
where α and β are fitting terms relating to chloride binding. As
Comb. Cl– ,SO42–
addition shown in Figure 9 in general, the Freundlich isotherm yielded
better fit of the experimental data and was selected for further
1,000 10,000 Figure 10 shows a compilation of chloride ion binding
isotherms for the laboratory-cast grouts. The data were parsed
by moisture content (delineating grout deficiency) and actual
free sulfate ion concentrations. The low and high sulfate levels
were defined by levels observed in as-received grouts (de-
fined earlier) and where corrosion developed (defined in the Risk
CORROSIONJOURNAL.ORG
 ENGINEERING SECTION

2
Moisture content <20%
Grout condition R2
Sulfate ions
Moisture SO4 Conc. Langmuir Freundlich
SO4 < 0.00042 gsulfate/ggrout
content gsulfate /ggrout isotherm isotherm
0.00042 < SO4 < 0.06 gsulfate/ggrout
SO4 < 0.00042 0.49 0.77 SO4 > 0.006 gsulfate/ggrout
<20% 0.00042 < SO4 < 0.06 0.86 0.77
Moisture content >20%
1.5 SO4 > 0.006 – –
Sulfate ions
SO4 < 0.00042 – –
SO4 < 0.00042 gsulfate/ggrout
>20% 0.00042 < SO4 < 0.06 0.31 0.43 0.00042 < SO4 < 0.06 gsulfate/ggrout
SO4 > 0.006 0.32 0.71 SO4 > 0.006 gsulfate/ggrout
CB (kg/m3)

0.5
Example data set
Freundlich isotherm (R2 = 0.7701)
Langmuir isotherm (R2 = 0.8640)

0
0 0.5 1 1.5 2
CF (kg/m3)
FIGURE 9. Comparison of Langmuir and Freundlich chloride ion binding isotherm.

4 0.5
Moisture content <20%
Sulfate ions
3.5 SO4 < 0.00042 gsulfate/ggrout 0.4
0.00042 < SO4 < 0.06 gsulfate/ggrout
SO4 > 0.006 gsulfate/ggrout
0.3
CB (kg/m3)

Moisture content >20%

3
Sulfate ions
SO4 < 0.00042 gsulfate /ggrout 0.2
2.5 0.00042 < SO4 < 0.06 gsulfate /ggrout
SO4 > 0.006 gsulfate /ggrout
CB (kg/m3)

0.1

2 0
0 0.1 0.2 0.3 0.4 0.5
CF (kg/m3)
1.5

0.5

0
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
CF (kg/m3)
FIGURE 10. Chloride ion binding isotherms for laboratory-cast hardened and deficient grout. Data with dotted outlines were considered outliers
and were not used for fitting. (Some of the low free chloride concentrations were considered as outliers due to relative error in the detection limit
of ion chromatography but otherwise still indicative of low chloride levels).

Assessment section), respectively. Figure 10 shows clear
differentiation in binding behavior between hardened and defi-
cient grout. Table 3 lists the binding isotherm fitting para-
meters. In general, notwithstanding possible negative effects of
sulfates, the alpha isotherm parameter was larger for hard-
ened grout than in the deficient grout and the beta isotherm
parameter varied for both hardened and deficient grout.
The alpha and beta isotherm parameters of the
Freundlich isotherm mathematically express scale (and op-
portunity) of the binding capacity of the material and the
shape of the isotherm (which may account for other material
parameters relating to chloride ion binding), respectively. It
was observed that the cement content was higher in the
hardened grout. With the higher cement factor, greater
availability of cement hydrates would enhance opportunity for
chloride binding. In contrast, the deficient grout had greater
water-to-cement ratio (less cement content), much greater
porosity, and large aggregation of silica fume which could
reduce overall chloride binding capacity.28,31-32 This would
be consistent with the larger alpha isotherm parameter in
hardened (nondeficient) grout. The observed variability in the
calculated beta isotherm parameter in both hardened and
deficient grouts likely relates to complexities in the grout such
as chloride transport to available interfacial sites between

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ENGINEERING SECTION

Table 3. Freundlich Isotherm Binding Coefficients

Freundlich Isotherm Fitting Parameters
Grout Condition α β R2
Moisture Content < 20% SO4 < 0.00042 gsulfate/ggrout 1.08 0.94 0.77
0.00042 < SO4 < 0.06 gsulfate/ggrout 0.74 0.65 0.77
SO4 > 0.006 gsulfate/ggrout No binding
Moisture Content > 20% SO4 < 0.00042 gsulfate/ggrout(A) — — —
0.00042 < SO4 < 0.06 gsulfate/ggrout 0.33 0.48 0.43
SO4 > 0.006 gsulfate/ggrout 0.34 0.88 0.71
(A)
Insufficient data available.

the C-S-H cement hydrates and the adjacent pore spaces tests and not to the amounts initially admixed to the grout.
complexation with C3A, and chloride binding in supple- Table A1 shows the measured free chloride and free sulfate
mentary cementitious materials.18,29-30,33 ion concentrations after testing and comparison to its premix
As shown in Table 3 for the hardened grout, the alpha design concentrations (shown in Tables 1 and 2). It is noted
isotherm parameter for chloride binding in grout with low sulfate that even though deficient grout was generated in the INT and
levels that developed from vestigial concentrations was ∼1.08. MIT tests, the quantities of deficient grout and thus the level of
With sulfate levels above this native concentration, the α term exposure of the steel corrosion probes in the deficient grout
was lower, 0.74. At high sulfate levels (>0.006 g/g), the limited varied. The results showed that sustained corrosion did not
available data showed indication for loss of binding capacity; always occur immediately after grout mixing; earlier findings
however, further verification is required. Nevertheless, the discussed in Part 2 suggested the importance of developed
data set is consistent with the literature, where sulfate presence grout resistance and grout hydration on corrosion rates.7 Indeed,
in cementitious materials was shown to reduce chloride ion corrosion initiation sometimes occurred after 100 d (particu-
binding capacity. In the deficient grout, chloride binding is already larly for the smaller INT samples). For comparison of the test
limited due to the low cement content, and the effect of sulfate cases, the terminal potentials and corrosion current densities
presence could not be clearly identified. were considered in the following.
Figures 11 and 12 show the cumulative fraction of INT
3.3 | Electrochemical Testing and MIT test specimen open-circuit potentials (OCP) (Ecorr) and
Figure A1 in the appendix shows the included test data for current density (icorr), respectively. Figure 11(a) shows data
OCP and icorr measured and calculated for all MIT and INT test from the INT test differentiating OCP for steel embedded in grout
specimen. These figures were included because subsequent from the tee header and the tee body. As expected, the
graphs and discussion derive from its contents. In the figure, due embedded steel probes in the hardened grout found in the tee
to the observed increase in ion concentrations in deficient body had passive potentials > −200 mVCSE. These potentials
grout, the data series were ordered based on the free chloride ion were consistent with the passive potentials for steel probes in a
and free sulfate ion concentrations measured at the end of the control grout mix. In some cases, for deficient grout found in

1 1
Hardened grout

0.9 0.9
(Tee body)

Deficient grout Hardened grout

(Tee header)
0.8 0.8
Cumulative Fraction

Cumulative Fraction

0.7 0.7
Deficient grout
0.6 0.6

0.5 0.5

0.4 0.4
Base: Base:
0.3 Na2SO4: 2,000 ppm 0.3 Na2SO4: 2,000 ppm
20,000 ppm 20,000 ppm
100,000 ppm–150,000 ppm 100,000 ppm–150,000 ppm
0.2 NaCl: 0.08 wt% cement 0.2 NaCl: 0.08 wt% cement
Cl– 0.2 wt% cement Cl– 0.2 wt% cement
0.1 Comb. Na2SO4 and NaCl: 0.1 Comb. Na2SO4 and NaCl:
Cl– 0.08 wt% cement: Cl– 0.08 wt% cement:
Control mix Cl– 0.2 wt% cement: Cl– 0.2 wt% cement:
0 0
0 –100 –200 –300 –400 –500 –600 0 –100 –200 –300 –400 –500 –600
Corrosion Potential (mVCSE) Corrosion Potential (mVCSE)
(a) (b)
FIGURE 11. Corrosion potential of steel in deficient grout. (a) INT test setup. (b) MIT test setup.

856 JULY 2019 • Vol. 75 • Issue 7 CORROSIONJOURNAL.ORG

 ENGINEERING SECTION

1 1

0.9 0.9
Hardened grout
0.8 0.8
Deficient grout

Cumulative Fraction
Cumulative Fraction

(Tee header) 0.7

0.7
Deficient grout
0.6 0.6
Hardened grout (Tee body)

0.5 0.5

0.4 0.4
Base: Base:
0.3 Na2SO4: 2,000 ppm 0.3 Na 2SO 4: 2,000 ppm
20,000 ppm 20,000 ppm
100,000 ppm–150,000 ppm 100,000 ppm–150,000 ppm
0.2 NaCl: 0.08 wt% cement 0.2 NaCl: 0.08 wt% cement
Cl– 0.2 wt% cement Cl– 0.2 wt% cement
0.1 Comb. Na2SO4 and NaCl:
Cl– 0.08 wt% cement:
0.1 Comb. Na 2SO 4 and NaCl:
Cl– 0.08 wt% cement:
Control mix Cl– 0.2 wt% cement:
Cl– 0.2 wt% cement:
0 0
0.0001 0.001 0.01 0.1 1 10 0.0001 0.001 0.01 0.1 1 10
Current Density (μA /cm2) Current Density (μA /cm2)
(a) (b)
FIGURE 12. Corrosion current density of steel in deficient grout. (a) INT test setup. (b) MIT test setup.

tee header, the potentials of the embedded steel also showed corrosion current densities were generally low, albeit elevated in
passive-like potentials even though physical and chemical comparison to steel embedded in the tee body. Nevertheless,
conditions (described above) gave indication of possible adverse there were several samples (with sulfate and combined sulfate/
corrosion environments. However, in the case of the combined chloride additions) in the tee header that exhibited high cor-
sulfate and chloride additions (2,000 to 20,000 sulfate with 0.08% rosion current densities (as high as 5 μA/cm2). In Figure 12(b),
to 0.2% chloride), more than 50% of the test probes had corrosion current densities for steel embedded in deficient
potential < −300 mVCSE, indicative of possible corrosion activity. grout in the upper elevations of MIT specimens were consistently
Figure 11(b) shows similar results for the MIT specimens, but and distinctly higher than in the hardened grout that formed in
the deficient grout in the upper duct elevation had more distinct the lower elevations of the MIT specimens (median values
differentiation of negative active potential, where 40% to 80% 0.005 μA/cm2 and 0.1 μA/cm2, respectively).
of the steel probes had potential < −300 mVCSE in grout with
2,000 to 20,000 sulfate and 0.08% to 0.2% chloride additions.
Figure 12(a) shows the icorr for INT specimens. There was 3.4 | Characteristic of Steel Corrosion Product
differentiation in the icorr values between the deficient and Examples of surface rust and localized corrosion on steel
hardened grout, consistent with the developed OCP for those embedded in lab specimens are shown in Figure 13. Figure 13(a)
cases. For the hardened grout in the tee body, the corrosion shows an area with mixed rust and residual grout material and
current densities were <0.003 μA/cm2, consistent with the Figure 13(b) shows a corrosion pit. EDS analysis showed the
expected low corrosion activity in the hardened grout and corrosion product contained iron and oxygen without clear
comparable to the low corrosion rates measured in control association with sulfur bearing species or chloride in its
grout mixes. Consistent with the passive-like OCP values for composition (Figure 14 and Table 4). The atomic and weight
some samples in the tee header that had deficient grout, the percentages of iron and oxygen was not inconsistent

4
2 1 1
2
3

250 μm 500 μm

(a) (b)
FIGURE 13. SEM micrographs of surface corrosion for steel embedded in deficient grout with combined admixed chloride and sulfate.
(a) Corrosion with grout. (b) Surface pitting.

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ENGINEERING SECTION

Full Scale Counts: 272 Point a1 Full Scale Counts: 292 Point a2
O
300 Fe Si
300 Ca
250
200 Fe
200
150 O Na
100 100 Fe
Mg
50 C S Cl Fe S Cl K
C Fe Fe
0 0
0 2 4 6 8 10 0 2 4 6 8 10
keV keV
Full Scale Counts: 282 Point a3 Full Scale Counts: 343 Point a4
CO
500 600 Ca
400 CO 500 Si
Si Fe Cl
Ca 400 S
300
Cl 300
200 Ca Na Si
S 200
Fe Fe Br
100 Na Si Ca
S 100 Mg
Mg Cl Fe S Cl K Fe Fe
0 0
0 2 4 6 8 10 0 2 4 6 8 10
keV keV
Full Scale Counts: 229 Point b1 Full Scale Counts: 229 Point b2
500 500 Si
Si
400 KO 400 C
C Fe KO
300 Ca 300 Cl Fe
Cl Ca
200 S Fe 200 S
Fe
100 Mg Ca 100 Na Ca
Na Si S Cl KK Fe Mg Si S Cl KK Fe
0 0
0 2 4 6 8 10 0 2 4 6 8 10
keV keV
Full Scale Counts: 245 Point b3

500 Si O
K Fe
400 Ca
C
300 Cl
200 S
Fe
100 Na Ca
Mg Si S Cl KK Fe
0
0 2 4 6 8 10
keV
FIGURE 14. EDS spectrum for steel embedded in deficient grout with combined admixed chloride and sulfate. (a) Corrosion with grout.
(b) Surface pitting.

with goethite for the surface rust and hematite in the
corrosion pit.34
3.5 | Risk Assessment
An important finding from laboratory-cast grout samples
was that the enhanced steel corrosion in presence of sulfate ions
occurred primarily in segregated grout, but corrosion activation
also occurred in deficient grout conditions that did not strongly
manifest physical segregated grout characteristics. In the defi-
cient grout, there is sufficient moisture with available free sulfates
from the initial grout injection. It was posed that significant early
free sulfate ion accumulation and availability of sufficient levels is
necessary to hinder stable steel passive film formation but
depassivation of steel by sulfates is otherwise difficult. The possible
role of sulfates in steel corrosion initiation were thought to be
related to localized corrosion process by reactions such as
Fe2þ þ 2H2 O þ SO2− 4 → FeðOHÞ2 þ H2 SO4 .
35
Furthermore, it
was posed that modest increase of chloride ion concentrations
(below conventional threshold concentrations) with elevated free
sulfate concentrations in the deficient grout can further aggravate
conditions resulting in early steel depassivation. Even though the
pH of the deficient grout was typically observed to be high, the
hydrolysis reaction would promote lower pH conditions in oc-
cluded regions perhaps such as in strand interstitial spaces.
The reduced presence of cement and the generally poor bulk
quality of the deficient grout could further allow development of
lower pH conditions by processes such as carbonation. Fur-
thermore, the lower cement content would minimize any interaction
of the free sulfates as well as chlorides with the cement during
hydration.

858 JULY 2019 • Vol. 75 • Issue 7 CORROSIONJOURNAL.ORG

 ENGINEERING SECTION

Table 4. EDS Elemental Analysis for Steel Embedded in Deficient Grout with Combined Admixed Chloride and Sulfate(A),(B)
at% Fe-K O-K C-K S-K Cl-K Ca-K Na-K K-K Mg-K Si-K Br-L
Point a1 27.84 45.88 26.28
Point a2 1.59 44.65 18.67 0.32 0.12 17.76 3.87 0.62 0.62 11.79
Point a3 9.43 52.84 26.00 1.36 0.02 7.78 1.22 0.01 1.34
Point a4 0.32 18.08 79.92 0.15 0.08 1.67 1.20 0.07 0.02 1.39 0.08
Point b1 32.24 49.14 16.62 0.12 0.12 0.92 0.24 0.61
Point b2 40.21 35.23 18.33 0.41 0.03 1.26 2.26 0.35 1.92
Point b3 49.43 22.82 22.29 0.16 0.31 2.34 1.39 0.32 0.08 0.87
wt% Fe-K O-K C-K S-K Cl-K Ca-K Na-K K-K Mg-K Si-K Br-L
Point a1 59.70 28.18 12.12
Point a2 4.02 32.28 10.13 0.46 0.19 32.16 4.02 1.09 0.69 14.97
Point a3 25.01 40.13 14.28 2.07 0.04 14.80 1.33 0.01 1.78
Point a4 1.28 20.94 66.85 0.36 0.20 4.86 2.00 0.20 0.04 2.83 0.44
Point b1 63.35 27.66 7.02 0.13 0.16 0.74 0.33 0.60
Point b2 69.88 17.54 6.85 0.40 0.04 1.57 1.62 0.43 1.68
Point b3 77.24 10.21 7.49 0.14 0.31 2.63 0.89 0.35 0.05 0.68
(A)
Point a1: corrosion; Point a2 and a3: surface with grout residue; and Point a4: sample surface.
(B)
Points b1 to b3: corroded surface.

The laboratory observations of steel corrosion in As a first approach to quantitatively characterize condi-
admixed sulfate solution tests with somewhat lower tions in deficient grout that can lead to corrosion, MIT and INT test
pH levels (pH ∼12.6) and corrosion development in strand results were compiled to differentiate the roles of moisture
embedded in the deficient grout soon after injection (where the content, free chloride content, and free sulfate concentrations on
grout pore water chemistry was still evolving) reflect early corrosion activity (characterized by Ecorr, icorr, and rust forma-
disruption to passive film growth. The lack of corrosion on tion). Figure 15 shows strong differentiation between the deficient
prepassivated steel with later incremental additions of sul- grout and hardened grout (characterized by its moisture con-
fates even up to high levels in both pH ∼13 and 12.6 solutions tent). The deficient grout (following earlier discussions) showed
furthermore would indicate that the mechanism of corrosion higher free sulfate concentrations and coincident active cor-
relates to the early instability of the steel passive film due to rosion potentials and higher corrosion rates of the embedded
early sulfate presence. The compounding effects from steel. Active corrosion potentials and enhanced corrosion rates
changes in the grout pore water chemistry should be further (and rust formation) were observed at free sulfate concentrations
evaluated. However, with a large existing bridge inventory36 as low as 0.0004 gsulfate/ggrout. That sample also coincided with
with similar grout materials in tendons that exhibited severe elevated free chloride concentrations. In general, corrosion ac-
corrosion,1 practical criteria to assess corrosion risk is tivity developed in grout with less than 420 ppm Cl− with free
needed to identify maintenance needs. sulfate concentrations >0.0007 gsulfate/ggrout.

0 10
Moisture content <20%
Free chloride:
Corrosion Potential (mVCSE)

Current Density (μA /cm2)

Cl– < 50 ppm

–100 1 50 ppm < Cl– < 420 ppm
Cl– > 420 ppm
Moisture content >20%
–200 0.1 Free chloride:
50 ppm < Cl– < 420 ppm No rust
Cl– > 420 ppm
No rust
–300 0.01
Moisture content <20%
Free chloride:
Cl– < 50 ppm
–400 50 ppm < Cl– < 420 ppm 0.001
Cl– > 420 ppm
Moisture content >20%
–500 Free chloride:
0.0001
50 ppm < Cl– < 420 ppm
Cl– > 420 ppm
–600 0.00001
0.00001 0.0001 0.001 0.01 0.1 0.00001 0.0001 0.001 0.01 0.1
Sulfate Concentration (gSO /ggrout) Sulfate Concentration (gSO /ggrout)
4 4
−
FIGURE 15. Corrosion behavior of steel in deficient grout with elevated sulfate concentration. 50 ppm Cl observed upper free chloride limit in
control hardened grout mixes. 420 ppm Cl− observed upper free chloride limit for segregated grout sans external chloride contaminants.
Dashed marker outlines denote conditions for observed corrosion. 0.0007 gsulfate/ggrout concentration shown as reference.

CORROSIONJOURNAL.ORG JULY 2019 • Vol. 75 • Issue 7 859

ENGINEERING SECTION
Changes in pore water chemistry can affect the initiation
of steel corrosion in the presence of sulfate ions. Earlier elec-
trochemical testing described in Part 1 of the series of papers
showed that steel in alkaline sulfate solution had dissimilar
corrosion behavior in simulated pore solutions with pH 12.6
and 13.3. It was therefore evident that defining propensity for
corrosion initiation in solution by free sulfate ion concentra-
tions alone may not be sufficient. For discussion, a ratio of
½SO2− −
4 =½OH  was adopted (Figure 16). The Ecorr and icorr of
steel in the different grout test conditions were compiled to
evaluate the influence of the combined factor of sulfate
concentration and pH (in pore water solutions with low-level
chloride ions) on corrosion development. Figure 16 shows
data for lab grout test samples and simulated pore solution tests.
Results for the grout samples were grouped by grout defi-
ciency (defined by moisture content) and free chloride levels
(defined by the upper chloride limits defined earlier). Test
specimens with grout conditions that were verified to have
developed surface rust on embedded steel probes were
separately demarcated. Samples that exhibited electrochemical
parameters characteristic to active corrosion are also marked.
The compilation of data from the MIT and INT tests, as
well as data from earlier testing in simulated pore water solution6
give general discrimination of corrosion activity due to the
higher ½SO2− −
4 =½OH  levels present in deficient grout. As seen in
Figure 16, active potentials ( ≤ 300 mVCSE) and higher corro-
sion current densities (>0.1 μA/cm2) were generally observed for
steel embedded in grout with higher moisture content and
−
higher ½SO2−4 =½OH . Similar to earlier discussion, it is noted that
these samples in deficient grout showed elevated chloride
levels relative to the hardened grout. Other samples with
−
somewhat elevated chloride levels but at lower ½SO2− 4 =½OH 
consistently showed passive corrosion conditions. Two samples
(free chloride concentration <50 ppm), with surface rust,
showed enhanced corrosion current density (icorr ∼0.3 μA/cm2)
with active corrosion potentials (Ecorr ∼−300 mVCSE) at
½SO2− −
4 =½OH ∼1. Two other samples (free chloride concentration
< 420 ppm) showed similar Ecorr and icorr values at
−
½SO2−
4 =½OH ∼0.15 but did not develop any significant levels of
surface rust during the time of the experiment. For compari-
son, free sulfate ion concentrations and leachate pH for grout
extracted from Florida bridges indicated that corrosion had
occurred in deficient grouts where the sulfate to hydroxyl ratio
exceeded 0.1.5 Corrosion testing in admixed sulfate solutions
0 10
Corrosion Potential (mVCSE)
–100
–200
Moisture content <20%
Free chloride:
Cl– < 50 ppm
–300 50 ppm < Cl– < 420 ppm
No rust
Cl– > 420 ppm
Moisture content >20%
–400 Free chloride:
50 ppm < Cl– < 420 ppm
Cl– > 420 ppm
Solution testing
–500 Admixed
pH 12.5
pH 13.3
Incremental
–600
0.0001 0.001 0.01 0.1 1 10
[SO42– ]/[OH– ] (mol/mol)
FIGURE 16. Corrosion behavior of steel in simulated and grout pore water solutions with elevated sulfate concentration. 50 ppm Cl− observed
upper free chloride limit in control hardened grout mixes. 420 ppm Cl− observed upper free chloride limit for segregated grout sans external
chloride contaminants. Dashed marker outlines denote conditions for observed corrosion. †: Data produced from testing described in Part 1 of
this series.6
860 JULY 2019 • Vol. 75 • Issue 7
(when steel prepassivation was not allowed) showed corrosion
development at sulfate to hydroxyl ratio greater than 0.7. But
solutions exceeding this ratio with pH 13 or any samples where
initial steel prepassivation was allowed did not develop cor-
−
rosion (even with ½SO2− 4 =½OH  as high as ∼10). It was evident
6
that the various test methodologies in grout and solution
can yield complications and the complexities of passive film
development should be examined in future work. Neverthe-
less, for the purposes of assessing the role of low-level
chlorides in the presence of elevated sulfate concentrations,
a ½SO2− −
4 =½OH  = 0.15 was nominally considered as a conservative
limit for corrosion in pore water solutions with chloride con-
centrations developed from vestigial chloride presence. At this
limit, the sulfate content in pH 12.6 to 13.3 pore solution
corresponds to ∼600 ppm to 3,000 ppm or 0.0007 gsulfate/ggrout
(generally consistent with the sulfate limits described earlier).
Figures 15 and 16 show that the largest corrosion rates
were measured for samples in deficient grout with the higher
levels of chlorides that developed from the initial low admixed
levels, 0.08 wt% and 0.2 wt%. It was necessary to elucidate the
role of low-level chlorides in the presence of elevated free
sulfate ion concentrations. To characterize sulfate ion concen-
trations that facilitate corrosion without the synergistic effect
of low-level chlorides, three levels were proposed based on
experimental observations. Low sulfate ion accumulation was
assumed to have concentrations less than 0.00042 gsulfate/ggrout,
which was the highest concentration of free sulfate measured
in the control base grout that did not have any grout degradation.
A proposed high-end value of 0.006 gsulfate/ggrout was based
on the sulfate concentration, where surface rust developed
during testing of steel in grout with Cl− levels < 50 ppm. The
intermediate sulfate range was proposed as characterizing
moderate free sulfate ion accumulation.
Figure 17 shows the Ecorr and icorr vs. total chloride
content from compiled tests results. Steel corrosion initiated, in
conditions where free sulfate ion concentrations exceeded the
low sulfate ion accumulation level defined above (regardless of
chloride ion concentrations developed from vestigial source
or admixed), as shown by the drop in corrosion potentials and
increase in corrosion rate. It is noted that the data points
representing samples that initiated corrosion37 placed within the
intermediate sulfate range (i.e., 0.0042 < sulfate concentration
< 0.006 gsulfate/ggrout) in Figure 17 typically had sulfate ion con-
centrations >0.0007 gsulfate/ggrout (as shown in Figure 15).
Moisture content <20%
Free chloride:
Cl– < 50 ppm
Current Density (μA /cm2)
1 50 ppm < Cl– < 420 ppm
Cl– > 420 ppm
Moisture content >20%
Free chloride:
0.1 50 ppm < Cl– < 420 ppm
Cl– > 420 ppm
Solution testing
No rust
0.01 Admixed
pH 12.5
pH 13.3
Incremental
0.001
0.0001
0.00001
100 1,000 10,000 0.0001 0.001 0.01 0.1 1 10 100 1,000 10,000
[SO42– ]/[OH– ] (mol/mol)
CORROSIONJOURNAL.ORG

0 10
Vestigal Cl–
Corrosion Potential (mVCSE)
–100
–200
–300
Moisture content <20%
Sulfate ions:
–400 SO4 < 0.00042 gsulfate/ggrout
0.00042 < SO4 < 0.006 gsulfate/ggrout
SO4 > 0.006 gsulfate/ggrout
Moisture content >20%
–500 Sulfate ions:
SO4 < 0.00042 gsulfate/ggrout
0.00042 < SO4 < 0.006 gsulfate/ggrout
SO4 > 0.006 gsulfate/ggrout
–600
0.00001 0.0001 0.001
Total Chloride Concentration (gCl/ggrout)
FIGURE 17. Corrosion behavior of steel in deficient grout with elevated sulfate and low-level of chloride. 0.00042 gsulfate/ggrout observed upper
sulfate limit in control hardened grout mixes. 0.006 gsulfate/ggrout observed upper sulfate limit for segregated grout where corrosion developed
with chloride less than 420 ppm, dashed marker outlines denote conditions for observed corrosion.
Samples with elevated free sulfate concentrations showed
an active icorr of ∼0.1 μA/cm2 (two magnitudes higher than passive
steel in grout with low free sulfate concentrations intrinsic to
nondeficient grout) at vestigial chloride content levels. The large
increase in corrosion current density was noted as significant
despite the generally low value because the calculated current
density would underestimate localized corrosion rates (such as
in the pitting observed in the field and laboratory samples).
It was apparent in those samples that the elevated
chloride concentrations (below conventional critical threshold
concentrations by cement mass8,14) in deficient grout can
significantly increase the corrosion rate of steel. The samples
with elevated sulfate concentration showed corrosion cur-
rents greater than 1 μA/cm2 when the chloride content exceeded
0.0003 gchloride/ggrout. These results would indicate that as-
sessment of corrosion susceptibility by chloride values alone in
deficient grout is insufficient as sulfate ion presence and grout
characteristics are also important.
The work at large described in the series of papers
sought to provide data to support recommendations relating free
sulfate ion concentrations in deficient grout and corrosion.
Test results have shown positive indication of corrosion acti-
vation of steel in solutions with free sulfate ions; however, the
challenge of providing a complete mechanistic description on
how sulfates disrupt passive film development at this time
remains elusive and conflicting experiences are disseminated in
the literature. Findings described in this paper also convey the
complications related to moderate increase of chloride ion
concentrations from vestigial concentrations in pre-
packaged grout.
Due to the serious consequence of the corrosion ex-
perienced in the field, it is necessary to establish practical
criteria for allowable levels of sulfate in the grout. Difficulty
with specifications relating to possible limits on free sulfate ion
concentrations in PT grouts lies in the fact that sulfur-
containing species are regularly part of cementitious materials.
The effect of limiting sulfates on the performance of the
material, especially in material specifications, should be
considered. Finally, much of the findings in the work relate
corrosion to the elevated presence of sulfates in deficient
grout. It was evident that elevation of sulfate ions is in part
due to transport of the ion to the areas of grout segregation.
Definitions of free sulfate ion concentration limits should
address that even low concentrations of free sulfates in
well hydrated grout may be locally increased due to
segregation.
CORROSIONJOURNAL.ORG
ENGINEERING SECTION
Moisture content <20%
Sulfate ions:
Admixed Cl–
Current Density (μA /cm2)
SO4 < 0.00042 gsulfate/ggrout
Passive37 0.00042 < SO4 < 0.006 gsulfate/ggrout
Enhanced
1 SO4 > 0.006 gsulfate/ggrout
Moisture content >20% corrosion
Sulfate ions:
SO4 < 0.00042 gsulfate/ggrout
0.00042 < SO4 < 0.006 gsulfate/ggrout
Intermediate 0.1 SO4 > 0.006 gsulfate/ggrout Activation
risk 37
0.01
High risk 37 0.001 Passive
Admixed Cl– Vestigal Cl–1
0.0001
0.01 0.00001 0.0001 0.001 0.01
Total Chloride Concentration (gCl/ggrout)
CONCLUSIONS
➣ Deficient grout was produced in laboratory specimens in
local regions with greater volume of displaced mix water. Higher
water-to-cement ratio, high pore content, and concentrated
agglomerations of silica fume particles were found in the
segregated grout. Furthermore, the grout segregation allowed
enhanced transport of sulfate and chloride ions.
➣ Physical and chemical deficiencies in segregated grout
(such as lower availability of hydrated cement, increase of free
sulfate ion concentration, and aggregation of silica fume)
reduced the extent of chloride binding. Although chloride binding
is already limited due to the low cement content in the defi-
cient grout, the result showed that sulfate presence in cemen-
titious materials may reduce chloride ion binding capacity.
➣ Elevated free sulfate ion concentrations had synergistic
effects with the chloride ion concentrations to reduce corrosion
resistance. Corrosion activity was shown to develop in grout
with elevated sulfate and native chloride concentrations.
However, it was shown that corrosion rates increased (greater
than 1 μA/cm2) for steel in deficient grouts (with the elevated sulfate
levels) due to elevated low-level chloride ions (below conven-
tional chloride threshold values). The moderate elevation of chloride
ion concentrations alone (without elevated sulfate levels) did not
create conditions to initiate corrosion activity. It was evident that
the assessment of corrosion susceptibility in deficient grout by
chloride values alone is insufficient as sulfate ion presence and
grout characteristics are also important. Due to the serious
consequence of the corrosion experienced in the field, it is nec-
essary to establish practical criteria for allowable levels of sulfate
in the grout. For this purpose, a limit of 0.0007 gsulfate/ggrout was
nominally proposed for controlling corrosion in cast grout.
ACKNOWLEDGMENTS
This investigation was supported by the Florida Department of
Transportation (FDOT). The opinions, findings and conclusions
expressed here are those of the authors and not necessarily
those of the FDOT or the U.S. Department of Transportation. The
contributions by Md. Ahsan Sabbir, Roberto Rodriguez, and Daniel
Yohannes are acknowledged here, as is the support and assistance
from the FDOT State Materials Office and Dr. H.R. Hamilton.
References
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with Deficient Grout: Corrosion Failure in Ringling Causeway
JULY 2019 • Vol. 75 • Issue 7 861
ENGINEERING SECTION
Bridge,” Florida Department of Transportation State Materials
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CORROSIONJOURNAL.ORG
 ENGINEERING SECTION

APPENDIX

0 Free chloride:
10 Free chloride:

Moisture
Moisture
c ontent

content
Cl– < 50 ppm Cl– < 50 ppm

>20%
>20%
50 ppm < Cl– < 420 ppm 50 ppm < Cl– < 420 ppm
Corrosion Potential (mVCSE)

Cl– > 420 ppm Cl– > 420 ppm

Current Density (μA /cm2)

–100 Free chloride:
1 Free chloride:

Moisture
Moisture
c ontent

content
Cl– < 50 ppm Cl– < 50 ppm

<20%
<20%
50 ppm < Cl– < 420 ppm 50 ppm < Cl– < 420 ppm
Cl– > 420 ppm Cl– > 420 ppm

–200
0.1
–300
0.01
–400

0.001
–500

–600 0.0001
0 50 100 150 200 250 300 350 400 0 50 100 150 200 250 300 350 400
Time (d) Time (d)
(a) (b)
0 Free chloride:
10 Free chloride:

Moisture
Moisture

content
Cl– < 50 ppm

>20%
content

Cl– < 50 ppm

>20%

50 ppm < Cl– < 420 ppm

Corrosion Potential (mVCSE)

50 ppm < Cl– < 420 ppm

Cl– > 420 ppm

Current Density (μA /cm2)

Cl– > 420 ppm
–100 Free chloride:
1
Free chloride:

Moisture
Moisture

content
Cl– < 50 ppm

<20%
content

Cl– < 50 ppm

<20%

50 ppm < Cl– < 420 ppm 50 ppm < Cl– < 420 ppm
Cl– > 420 ppm Cl– > 420 ppm

–200
0.1
–300
0.01
–400
0.001
–500

–600 0.0001
0 50 100 150 200 250 300 350 400 0 50 100 150 200 250 300 350 400
Time (d) Time (d)
(c) (d)
0 10 Free chloride:

Moisture
Free chloride:

content
Moisture

Cl– < 50 ppm

>20%
content

Cl– < 50 ppm

>20%

50 ppm < Cl– < 420 ppm 50 ppm < Cl– < 420 ppm
Corrosion Potential (mVCSE)

Cl– > 420 ppm Cl– > 420 ppm

Current Density (μA /cm2)

–100 Free chloride: Free chloride:

Moisture
1
content
Moisture

Cl– < 50 ppm

<20%
content

Cl– < 50 ppm

<20%

50 ppm < Cl– < 420 ppm 50 ppm < Cl– < 420 ppm
Cl– > 420 ppm Cl– > 420 ppm

–200
0.1
–300
0.01
–400

0.001
–500

–600 0.0001
0 50 100 150 200 250 300 350 400 0 50 100 150 200 250 300 350 400
Time (d) Time (d)
(e) (f)
FIGURE A1. OCP and corrosion current for INT and MIT samples. (a and b) SO2−
4 < 0.00042 g=g. (c and d) 0.00042 < SO2−
4 < 0.006 g=g.
(e and f) SO2−
4 > 0.006 g=g.

CORROSIONJOURNAL.ORG JULY 2019 • Vol. 75 • Issue 7 863

 Table A1. Grout Sulfate, Chloride, Moisture, and pH Levels for MIT and INT Test Cases
Sulfate Content Total Chloride
(mgsulfate/gpowder) Free Chloride (ppm) (mgchloride/gpowder) Moisture Content (%) pH of Leachate

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Bottom Bottom Bottom Bottom Bottom
Sample Cases Top Section Section Top Section Section Top Section Section Top Section Section Top Section Section
MIT Base 23–24 0.4 150–158 13–22 0.1–0.2 0.1 61–67 13–14 10–10.7 12.4
MIT Sulfate-1 0.1–0.7 0.4 70–122 36–176 0.1 0.1 16–18 12–13 12.5–12.6 12.5
MIT Sulfate-2 0.1–40 0.5 38–250 10–18 0.1–0.2 0.1 14–61 10–18 12–12.9 12.8
MIT Sulfate-3 6.6–7 4.4–6.8 38–24 28–40 0.1 0.1 15 14–13 12.6 12.5–12.6

864 JULY 2019 • Vol. 75 • Issue 7

ENGINEERING SECTION

MIT Chloride-1 1–16 0.5 880–1,520 162–182 1.1–1.3 0.4–0.5 31–38 12–11 12–12.5 12.4
MIT Chloride-2 0.4–1 0.6 620–1,800 500–560 1.9–2.6 1 17–31 11 12.5–12.6 12.5
INT Ctrl Base 0.1–0.2 0.2 54–60 56–50 0.2 0.1 10–11 12 12.8 12.7
INT Ctrl Sulfate-1 0.1–0.2 0.2–0.3 54–104 50 0.2 0.1 11 12 12.8 12.7
INT Ctrl Sulfate-2 0.4–0.5 0.3–0.4 80–68 50 0.1–0.2 0.1 11 12–13 12.8 12.7
INT Test Base 0.3–1 0.2–0.3 74–112 50–58 0.1–0.3 0.1 21–25 10–15 12.4–12.7 12.7–12.8
INT Test Sulfate-1 1.4–12 0.2–0.3 112–176 50–68 0.2–0.3 0.1 30–41 12–14 11.2–12.4 12.7–12.8
INT Test Sulfate-2 13–20 0.2–0.3 144–260 50 0.2–0.3 0.1 25–43 10–12 11.4–11.9 12.8
INT Test Sulfate-3 3.4–6.4 0.3–2.2 64–102 50–420 0.1–0.2 0.1 14–18 14–16 12.7 12.8
INT Test Chloride-1 2 1.8–1.9 340–400 140–130 0.6–0.7 0.4 17–23 11–13 12.6 12.7
INT Test Chloride-2 1.9 0.4–3.6 620–640 5–50 1.2–1.3 0.9–1 18–19 13–16 12.7 12.7
INT Test Combined-1 10.4–14.8 0.2–0.3 560–680 104–132 0.3–0.4 0.2–0.4 53 9–11 11.3–11.7 12.7
INT Test Combined-2 12–2 0.4 980–1,520 162–174 0.6–0.8 0.3–0.4 52–60 10 11.4–11.6 12.7
INT Test Combined-3 3.6–4.2 3.4–3.6 240–260 220–240 0.5 0.4–0.5 16–17 16/16 12.9 12.9
INT Test Combined-4 1.1–32 0.3 1,640–1,200 260–360 0.6–1 0.6–0.8 51–57 9/10 11.3–11.8 12.7
INT Test Combined-5 14–19.4 0.4–0.6 1,400–2,200 300–520 1.6–1.8 0.7–0.9 47–50 11/20 11.7 12.8
INT Test Combined-6 4.8–5.6 3.8–4 660–740 580 0.9–1 0.8–0.9 17–18 16/15 12.9 12.7

CORROSIONJOURNAL.ORG