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Cement and Concrete Composites 107 (2020) 103491

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Cement and Concrete Composites


journal homepage: http://www.elsevier.com/locate/cemconcomp

Relating water permeability to electrical resistivity and chloride


penetrability of concrete containing different supplementary
cementitious materials
Caitlin M. Tibbetts a, Jerry M. Paris a, Christopher C. Ferraro a, *, Kyle A. Riding a,
Timothy G. Townsend b
a
Department of Civil and Coastal Engineering, University of Florida, P.O. Box 116580, Gainesville, FL, 32611, USA
b
Department of Environmental Sciences, University of Florida, P.O. Box 116450, Gainesville, FL, 32611, USA

A R T I C L E I N F O A B S T R A C T

Keywords: Electrical test methods for predicting concrete penetrability have been widely accepted for use in assessing
Concrete quality and durability of concrete; however, these methods are indirect and have not been related to concrete
Water permeability water permeability. This research compares three standardized electrical test methods, AASHTO T 358, AASHTO
Electrical resistivity
TP 119, and ASTM C1202, to hydraulic/water permeability. As no consensus standardized water permeability
Chloride ion penetrability
test method is available, a uniaxial, steady-flow permeameter test that has generally been used within the
Pore solution
Supplementary cementitious materials research community was employed for this research. The results demonstrate that the electrical test methods
investigated for predicting concrete penetrability are not necessarily appropriate for concrete mixtures con­
taining alternative supplementary cementitious materials. Materials with electrically conductive components in
pore solution or bulk matrix perform poorly in electrical testing such as surface or bulk resistivity, or chloride ion
penetrability testing, although water permeability indicates comparable performance to traditional supple­
mentary cementitious materials.

1. Introduction serviceability and durability of concrete structures as most degradation


processes are dependent on the movement of fluid within the pore
A durable concrete must possess the ability to withstand weathering, structure [1–7]. Degradation mechanisms including corrosion of rein­
chemical attack, abrasion, and other degradation mechanisms during forcing steel, freeze-thaw, chemical attack, alkali-silica reactivity, and
the designed service life and exposure conditions while maintaining an carbonation are related to the penetrability and saturation level of the
acceptable level of operation [1]. The long-term durability of concrete is concrete. The ability of concrete to resist penetration of substances
one of the most important properties when designing concrete structures (e.g., water, chloride ions) depends on the porosity and pore charac­
for their intended service life. Exposure sites for durability specimens teristics of the matrix [8–10]. The porosity and pore structure devel­
are valuable for assessing performance in real exposure conditions; opment of concrete are influenced by several factors including:
however, exposure sites typically require long exposure times, which are materials, concrete mixture design, admixtures, curing practices, age,
unacceptable for most material qualification testing. Therefore, and construction techniques [4,10–14]. Research has shown that the
short-term test methods are needed to predict durability for the water-cementitious (w/cm) ratio strongly affects the permeability of
constantly evolving concrete industry. The use of alternative supple­ concrete [6,9–11,15]. The total cementitious content and use of sup­
mentary cementitious materials (SCMs), innovative admixtures, and plementary cementitious materials also plays a major role in the hy­
complex concrete mixture designs make it impractical to rely on expo­ dration and penetrability of concrete [4,11,14–16]. Older, more
sure sites for qualifying concrete. hydrated concrete will possess a more developed pore structure and
Research has shown that the transport properties (e.g., permeability, lower permeability [4,6,10]. Concrete containing SCMs will generally
diffusivity, absorption/sorption) of concrete are indicators of the have delayed hydration, thus more time is required to develop resistance

* Corresponding author.
E-mail addresses: ctibbetts@ufl.edu (C.M. Tibbetts), jerry.paris@essie.ufl.edu (J.M. Paris), ferraro@ce.ufl.edu (C.C. Ferraro), kyle.riding@essie.ufl.edu
(K.A. Riding), ttown@ufl.edu (T.G. Townsend).

https://doi.org/10.1016/j.cemconcomp.2019.103491
Received 12 April 2019; Received in revised form 2 August 2019; Accepted 19 December 2019
Available online 23 December 2019
0958-9465/© 2019 Published by Elsevier Ltd.
C.M. Tibbetts et al. Cement and Concrete Composites 107 (2020) 103491

to permeation [4,16]. The concrete pore structure is a dynamic system as the resistance. Bulk resistivity passes the current through the entire
it changes with the hydration process and deterioration from exposure specimen from end to end using stainless steel plates as electrodes
conditions. Cement hydration products form in the void spaces pro­ connected to the Wenner probe tips. First principles using Ohm’s law
ducing a denser pore structure, whereas degradation mechanisms cause relate the total charge passed from CIP to the bulk resistivity of the
internal damage and often lead to cracking. As a result, measurements of material as given in Eq. (1) [17,28,33,34]. The final numerator of Eq. (1)
concrete transport properties are a function of the testing parameters, assumes the standard testing voltage of 60 V, a testing period of 6 h, and
sample conditioning, and type of transport mechanism being measured a specimen geometry of 102 mm � 50 mm.
[3]. Z 6 ​ hr Z 6 ​ hr
V A A 1 21; 180
Many test methods have been developed to estimate the transport Q¼ I dt ¼ dt ¼ V t ¼ (1)
properties of concrete, ranging from long-term exposure tests to elec­ 0 ​ hr 0 ​ hr ρ L L ρ ρ
trical resistivity test methods. As electrical resistivity methods have
where Q ¼ total charge passed from CIP (coulombs).
become more widely used, there is a need to evaluate the reliability of
using these methods as a tool for rating concrete water permeability.
V ¼ test voltage (V)
This research focused on analyzing the relationship between standard­
L ¼ thickness of the specimen (cm)
ized electrical test methods for estimating concrete penetrability and
A ¼ cross-sectional area of the specimen (cm2)
pressurized hydraulic/water permeability.
t ¼ test period (s)
ρ ¼ bulk resistivity (kΩ-cm)
1.1. Electrical test methods for predicting concrete penetrability
Sample conditioning for surface and bulk resistivity test methods has
To answer the demand from industry to have an alternative to long-
been identified as very important for accurate measurement; tempera­
term exposure tests for determining concrete transport properties,
ture and degree of saturation of the samples can have a significant in­
electrical test methods were developed. In the 1980s ASTM C1202
fluence on the results [4,5,15,26–28,33,35–38]. The specimen geometry
(AASHTO T 277) became the first electrical test method for predicting
also affects the measured resistivity, and the bulk resistivity results must
concrete penetrability to be widely adopted [6,17–19]. Although origi­
be corrected for specimen dimensions. While the surface and bulk re­
nally termed the rapid chloride permeability (RCP) test [19], it was later
sistivity test methods are related to the penetrability, they are indirect
revised by ASTM to the “Standard Test Method for Electrical Indication
methods influenced by factors other than the physical pore matrix
of Concrete’s Ability to Resist Chloride Ion Penetration” or as referred to
characteristics. Resistivity measurements can be affected by the source
herein as the chloride ion penetration (CIP) test [17]. The method in­
of cement and SCMs and their chemical makeup as well as chemical
volves cutting and sealing the specimens before an electrical potential of
admixtures [1,17,27,28,37].
60 V is applied across the ends of the specimen for 6 h while the total
Similar to the CIP test, surface and bulk resistivity are also influenced
charge (in coulombs) passed through the specimen is measured. The
by the resistivity of the pore solution [1,33,38,39]. In an attempt to
total charge passed is a measure of the electrical conductance of the
account for this effect, the pore solution can be expressed from speci­
concrete and was related to measurements of chloride intrusion from
mens and tested for resistivity. Several devices for pore solution
long-term ponding tests (AASHTO T 259) [20]. The results were used to
expression have been developed; however, the process can be time and
establish a table that classifies the concrete chloride ion penetrability
labor intensive as pore solution expression requires large compressive
from high to negligible based on charge passed [17,19,20]. This method
forces to drive the fluid out of the pores of the specimen [40–42]. As a
has been criticized for not truly measuring the penetrability of concrete
result, pore solution expression is commonly performed on cementitious
because the current flow is also a function of the pore solution con­
paste specimens as the force required is lower due to the absence of
ductivity [3]. Additional criticism has been expressed as the method is
aggregate that usually has a higher modulus of elasticity and low ab­
time consuming, destructive, prone to errors from sample heating, and
sorption. The pore solution resistivity can also be estimated using online
fails to account for the differences in chemistry due to the inclusion of
calculators and equations that use cementitious material composition
SCMs [21–25]. Despite the shortcomings, the CIP test has been used for
and degree of hydration for commonly available materials [38,43–45].
over 30 years and is still used as an index test for concrete penetrability.
The pore solution composition primarily consists of sodium (Naþ), po­
Although it has been standardized and widely used to evaluate
tassium (Kþ), calcium (Ca2þ), and hydroxide ions (OHˉ), where Naþ, Kþ,
durability in concrete, the CIP test is an indirect method of measuring
and OHˉ concentrations predominantly control the conductivity and pH
the penetrability or flow properties of concrete. The CIP test method is
values [1,39–44]. There are a number of other minor ions that
much shorter compared to traditional long-term tests that directly
contribute to the pore solution composition and affect its properties, but
measure the transport properties of concrete, but it requires extensive
the reactions are more complex and less understood [46].
sample preparation and equipment. Research has thus been focused on
the development of more rapid test methods that correlate well with the
established CIP test. Extensive research has been conducted on short- 1.2. Water permeability test methods
term electrical resistivity testing and two methods have been stan­
dardized [4,5,15,26–28]. Surface resistivity (AASHTO T 358) and bulk Although the dominant transport mechanism in a concrete structure
resistivity (AASHTO TP 119) were developed as rapid methods for depends on the exposure conditions and saturation level in the concrete
qualifying the degree of concrete penetrability and have been stan­ matrix, the water permeability test is a direct method and is able to
dardized by the American Association of State Highway and Trans­ measure the interconnectivity of the pore structure. Research and case
portation Officials (AASHTO) [27,28]. The bulk resistivity test was studies have shown that permeability is one of the most important
made a provisional standard in 2015 by the Department of Trans­ characteristics for predicting concrete durability [7,47]. Consequently,
portation (DOT) community (AASHTO), but has not been adopted there has been considerable interest in measuring the water perme­
through a process of consensus outside of the DOT community [28–30]. ability of concrete, and research involving pressure driven flow has been
Surface and bulk resistivity are also indirect, electrically-based methods conducted for over 125 years [6,9,12,47–70]. Some non-consensus,
of measuring concrete durability; however, both are simple tests that standardized test methods exist [55–58,69], but there is no consensus
can be performed within minutes, making them ideal for routine standardized testing procedure for measuring water permeability
acceptance testing [31,32]. available today. Many researchers have thus developed their own
Surface resistivity applies a current across the surface of the spec­ testing method, with the majority of methods employing uniaxial flow
imen using a Wenner probe and measures the voltage drop to calculate [53,56–61,69–71]. While the exact equipment and procedures vary by

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C.M. Tibbetts et al. Cement and Concrete Composites 107 (2020) 103491

researcher, the basic principles are the same; a pressure gradient is relationships between each are evaluated. The pH and conductivity of
applied to a concrete specimen and the resulting flow rate is measured. the pore solution were measured to investigate the influences on the
Assuming laminar flow through a saturated porous medium, Darcy’s law electrical test methods.
is used to calculate the coefficient of permeability based on Eq. (2) [1,3,
60,65,68]. 2. Material and methods
QL
K¼ (2) 2.1. Mixture design
AP

where K ¼ water permeability coefficient (m/s). Nineteen concrete mixtures were investigated for this study; mixture
proportions are provided in Table 1. Cementitious materials for this
Q ¼ flow rate through the specimen (m3/s) research study included: Type I/II ordinary portland cement (OPC),
L ¼ thickness of the specimen (m) Class F fly ash (F), Class C fly ash (C), silica fume (SF), ground granulated
A ¼ cross-sectional area of the specimen (m2) blast furnace slag cement (Slag), metakaolin (MK), ground glass (GG),
P ¼ hydraulic pressure drop over the specimen expressed as equiv­ and three types of sugarcane bagasse ashes (SCBA). The number in the
alent pressure head (m) mixture name represents the percent portland cement replacement for
the particular supplementary cementitious material. The chemical
For this research study, a constant pressure, uniaxial, steady-state composition was measured using x-ray fluorescence for the cementitious
flow permeameter was used, similar to other water permeability test materials and is provided in Table 2.
setups seen in the literature [53,59–61,71]. The setup was developed at The mixtures with sugarcane bagasse ash denoted as “SCBA” repre­
the University of Florida in the late 1980s to provide a reliable, efficient, sent material originally acquired for testing, whereas mixtures denoted
and easy-to-replicate method for determining the water permeability of either “SCBA-A” or “SCBA-B00 represent additional materials obtained
concrete specimens [53,72]. from a facility with an older incineration process (older boiler type and
Water permeability measurements of concrete can have high vari­ emission controls, similar to SCBA) and a newer, more efficient incin­
ability and require care to obtain accurate results, but can give an eration process, respectively. The relatively high levels of phosphorus,
indication of the interconnectivity of the capillary pores and the quality P2O5, (2–7% by mass) and potassium, K2O, (2–6% by mass) are attrib­
of concrete [47,53,54,60,61,72,73]. Some of the variability, especially uted to fertilizer as they represent two of the three primary nutrients
at early ages, is due to the continued hydration of the specimens during used in fertilizer [74,75]. These elevated levels have been seen in other
testing; this can make it difficult to reach steady-state flow [3,54,73]. studies incorporating agricultural waste [70,76–80]. Sugarcane bagasse
The advantage of the saturated water permeability test is that it directly ashes have shown promising strength properties, but little research has
measures permeability through Darcy’s law and only measures one been done on the effect of SCBA cement replacement on the transport
transport mechanism, whereas other tests can be a combination of properties of concrete [76–79,81–89]. It should be noted that based on
diffusion, absorption, or permeability. The specimen conditioning and the chemical composition, the sugarcane bagasse ashes investigated in
testing procedure minimize effects of binding that can occur when using this study could not be classified as a Class N pozzolans according to
solutions (sodium chloride) and do not require specimen drying that is ASTM C618 without further processing [90].
known to alter the pore structure [1]. The coarse aggregate used was Florida limerock with No.89 grada­
This study investigated the relationship between electrical test tion and saturated surface-dry (SSD) specific gravity of 2.39; Florida
methods for predicting penetrability (AASHTO T 358, AASHTO TP 119, limerock is more porous, less dense, and softer than typical limestone
and ASTM C1202) and water permeability. The objective was to deter­ found in other regions [91–93]. The fine aggregate was a quarzitic sand
mine the reliability of the electrical test methods for estimating dura­ with a fineness modulus of 2.45 and SSD specific gravity of 2.62. The
bility of concrete containing a variety of supplementary cementitious ratio of fine to total aggregate volume was 0.5 for each of the concrete
materials. Although electrical test methods have been related to long- mixes.
term ponding and diffusion tests, a comparison to water permeability Mixing was performed in general accordance with ASTM C192 using
has not yet been performed and the effect of a broad range of SCMs on a drum mixer [94]. Specimens were cast into 102 mm � 205 mm cyl­
the electrical resistivity has not been established. The results obtained inders, immediately covered with plastic to prevent moisture loss, and
from electrical test methods and water permeability and the then demolded after 24 h. Following demolding, specimens were

Table 1
Concrete mixture proportions (kg/m3).
No. Mixture w/cm Portland cement Repl. 1 Repl. 2 Water Fine aggregate Coarse aggregate

1 OPC – Control 0.37 534 – 198 795 724


2 20F 0.37 427 107 198 780 711
3 20C 0.37 427 107 198 787 717
4 7SF 0.37 497 37 198 788 718
5 50Slag 0.37 267 267 198 786 717
6 20F/50Slag 0.37 160 107 267 198 771 702
7 10MK 0.37 481 53 198 785 716
8 10SCBA 0.37 481 53 198 783 714
9 20C/10SCBA 0.37 374 107 53 198 775 707
10 7SF/50Slag 0.37 230 37 267 198 779 710
11 20C/50Slag 0.37 160 107 267 198 778 709
12 30C/5F 0.37 347 160 27 198 778 710
13 20GG 0.37 427 107 198 784 714
14 20C/5GG 0.37 400 107 27 198 784 714
15 20SCBA 0.37 427 107 198 772 704
16 20SCBA-A 0.37 427 107 198 783 713
17 20SCBA-B 0.37 427 107 198 779 710
18 10SCBA-A 0.37 481 53 198 788 719
19 10SCBA-B 0.37 481 53 198 787 717

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Table 2
Chemical composition of materials by x-ray fluorescence.
Chemical oxide OPC F C SF Slag MK GG SCBA SCBA-A SCBA-B

SiO2 18.7 57.8 34.7 90.9 33.6 51.5 71.9 58.7 67.0 40.8
Al2O3 5.36 21.4 18.5 0.39 14.4 43.7 0.48 1.66 1.32 1.37
Fe2O3 4.44 11.8 5.66 2.14 0.61 0.47 0.10 2.52 2.98 2.78
CaO 63.5 1.29 26.4 0.85 41.1 <0.01 9.21 20.8 17.0 35.9
MgO 0.94 1.32 6.36 0.78 5.88 0.14 4.11 4.10 3.17 3.94
SO3 3.27 0.24 1.84 <0.01 2.56 0.01 0.20 3.00 0.92 4.60
Na2O 0.14 0.90 1.88 0.20 0.19 0.28 12.9 0.41 0.23 0.46
K2O 0.40 2.52 0.43 1.07 0.34 0.25 0.05 1.86 2.31 6.14
TiO2 0.27 0.99 1.45 <0.01 0.53 1.35 0.01 0.10 0.15 0.12
P2O5 0.64 0.19 0.86 0.10 0.02 0.08 <0.01 6.72 4.46 2.42
Mn2O3 0.07 0.04 0.04 0.19 0.35 <0.01 <0.01 0.16 0.13 0.08
SrO 0.07 0.05 0.43 0.01 0.07 0.02 0.01 0.14 0.15 0.24
Cr2O3 0.07 0.02 0.01 <0.01 <0.01 0.01 <0.01 0.02 0.04 –
ZnO 0.08 0.02 0.01 0.07 <0.01 <0.01 <0.01 0.07 0.05 0.08
BaO – 0.07 0.83 <0.01 0.06 0.20 <0.01 – 0.06 0.06
Total 98.0 98.7 99.4 96.7 99.7 98.0 99.0 100 99.9 99.0
LOI 2.80 1.16 0.21 4.18 0.95 1.46 0.41 42.0 24.4 12.4
Na2Oeq 0.40 2.56 2.16 0.90 0.41 0.44 12.9 1.63 1.75 4.50

submerged in a saturated limewater tank kept at 23.0 � C � 2.0 � C until 2.2.2. Pore solution expression
test preparation. The pore solution for this study was expressed from cementitious
Pore solution analysis was conducted on cementitious paste speci­ paste specimens that were representative of the concrete mixtures
mens that were representative of the first fifteen concrete mixtures in excluding SCBA-A and SCBA-B. The specimens for pore solution analysis
Table 1; SCBA-A and SCBA-B materials were not analyzed. Cementitious were vacuum-sealed and stored in a temperature-controlled room at
paste mixing was performed in accordance with ASTM C305 [95]. 23.0 � C � 2.0 � C until testing age. At ages of 28 and 56 days, the spec­
Specimens were cast into approximately 50 mm � 75 mm cylinders, imens were removed from sealed bags and placed in a pore solution
cured 24 hours, demolded, then immediately vacuum-sealed in a damp expression device as shown in Fig. 1, similar to the one described by
paper towel to prevent leaching and moisture loss. The sealed specimens Barneyback and Diamond [42]. The specimens were placed in the device
were stored in a temperature-controlled room at 23.0 � C � 2.0 � C until whole instead of crushed to minimize moisture loss and carbonation.
testing age. The pore solution from sealed specimens will have different The pore expression device confines the specimen while it is loaded in
alkali concentrations than the concrete specimens cured in saturated compression to extract the fluid from the pores. The groove in the bot­
limewater due to differences in degree of hydration and leaching; tom platen collects the pore fluid and connects to a drain on the side of
however, research has shown good correlation between measured and the base. The resultant solution was collected from the drain in a vial
theoretical estimates of pore solution conductivity, for sealed specimens and immediately tested for pH and conductivity.
[33,36,38].
2.2.3. Water permeability
Specimens were cut as 50 mm slices from the middle of each 102 mm
2.2. Experimental setup � 205 mm cylinder. The sides of the specimens were roughened slightly,
while not damaging or changing the dimensions of the specimen, to
2.2.1. Electrical test methods create an abraded surface for bonding of the epoxy sealant. Loose par­
Surface resistivity (SR) and bulk resistivity (BR) were measured in ticulates were removed, and the exterior of the specimens was dried. To
accordance with AASHTO T 358 and AASHTO TP 119, respectively [27, seal the sides against the pressurized water flow, the water permeability
28]. Before testing, the ends of the cylinders were ground flat to provide specimens had a 25 mm ring of epoxy formed around the specimens; the
better contact for bulk resistivity measurements, and the diameter and epoxy ring restricted flow through the faces of the specimens and pro­
length were measured to correct for geometry. The cylinders were stored vided a bearing surface for sealing the specimens while under pressure.
submerged in saturated limewater tanks until time of testing and were Soongswang et al. [53] details the procedure for specimen preparation
marked at each quadrant so that the probe placement for the surface for the water permeability test. Subsequent to the epoxy curing, the
resistivity test was consistent. Lime-saturated cloth squares were used as specimens were vacuum saturated according to ASTM C1202 [17]; this
the conductive medium between the specimens and the stainless steel saturation technique was adopted to be consistent with the preparation
plate electrodes for bulk resistivity measurements to provide good of the CIP specimens and to decrease the time required to achieve
electrical contact. To reduce variability, the cylinders were tested at steady-state for water permeability. After vacuum saturation was com­
23.0 � C � 2.0 � C and kept saturated during testing per AASHTO T 358 plete, the specimens were assembled in permeameter cells as shown in
and AASHTO TP 119 [27,28]. Fig. 2.
The specimens for chloride ion penetrability (CIP) were tested in Each permeameter cell was attached to a manometer tube that
accordance with ASTM C1202 [17]. Specimen preparation included the connects to a calibrated measuring board as shown in Fig. 3. The top and
acquisition of 50 mm slices from the middle of each 102 mm � 205 mm bottom chambers of the permeameter cell were filled with water so that
cylinder to produce representative samples of the bulk concrete. The both sides of the specimen were kept saturated and the top chamber was
specimens were then sealed on the sides with epoxy and vacuum satu­ pressurized. A reference cell was also assembled to account for the effect
rated according to the conditioning procedure in ASTM C1202 [17]. The of temperature and evaporation on the manometer tube reading. The
conditioning procedure for vacuum saturation involved: placing the reference cell contained no test specimen and had a solid base acrylic
specimens in a desiccator with the faces exposed, maintaining a mini­ plate (no hole), creating a zero-flow condition.
mum vacuum of 28 inches Hg for 3 hours, then covering with water while A gauge pressure of 586 kPa was used for the duration of testing and
still under vacuum for an additional hour, and finally removing vacuum the water level drop in the manometer tubes was measured over time.
and keeping specimens submerged under water for 18 � 2 hours. After The rate of water flow through the specimen was calculated by
vacuum saturation, specimens were assembled into the CIP cells using the measuring the water level drop in the manometer tube for the specimen
rubber gasket alternative and secured with bolts and tested [17].

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C.M. Tibbetts et al. Cement and Concrete Composites 107 (2020) 103491

Fig. 1. Diagram of pore solution expression device.

sufficiently to produce calcium hydroxide for the reaction [1,96]. Dif­


ferences in the rate of pozzolanic reactivity were observed between the
various SCMs investigated in this study; mixtures containing fly ash had
a delay in electrical resistivity development, while mixtures containing
silica fume and metakaolin reacted quickly and had large increases in
electrical resistivity at early ages.
The only mixtures that did not outperform the control at 56 days
were binary sugarcane bagasse ash mixtures, which had low surface and
bulk resistivity values overall but performed slightly better in bulk re­
sistivity with only two mixtures not exceeding the control at 56 days.
The two mixtures with the highest surface and bulk resistivity were
7SF/50Slag followed by 20F/50Slag. However, 10MK had higher initial
Fig. 2. Diagram of water permeability cell with concrete specimen cast in resistivity at 7 and 28 days; all three mixtures had equivalent penetra­
epoxy ring. bility classification of “very low” at 56 days per AASHTO T 358 and TP
119 [27,28]. These SCMs or combination of SCMs are known to have
and subtracting the water level drop for the reference cell over time. high pozzolanic reactivity, making them beneficial for concrete struc­
Water permeability specimens were tested for approximately two to tures in aggressive environments [1,40,46,97]. Due to the high surface
three weeks to achieve steady-state condition; permeability was calcu­ area of silica fume and metakaolin, the hydration rate is faster
lated from the average flow rate after steady-state was achieved. Steady- contributing to the early resistivity. It is important to note that the
state flow can be reached in days or weeks depending on the quality of standard curing age for many tests is 28 days based on traditional
the concrete and degree of hydration [53,72]; concrete mixtures with a mixture designs with portland cement, but with the inclusion of SCMs
low w/cm or specimens that have an advanced curing age, will generally and advances in binary and ternary mixture designs, a curing period of
take longer to achieve steady-state flow. 56 days is recommended to gain the benefits of a more developed pore
structure from the pozzolanic reaction [17].
3. Results and discussion The surface resistivity versus bulk resistivity results are plotted in
Fig. 4 with a linear regression line through the origin. There is a strong
3.1. Surface and bulk resistivity linear correlation between the surface and bulk resistivity measure­
ments, with an overall R2 value of 0.99 and a slope of 1.93 for a total of
Surface and bulk resistivity were measured at 7, 28, 56, 91, 182, and 95 data points (average of three specimens). The ratio between the
up to 365 days according to AASHTO T 358 and TP 119, respectively surface and bulk resistivity measurements (1.93) is in agreement with
[27,28]. Surface resistivity results were multiplied by 1.1 due to lime­ the geometry correction factors proposed by Morris et al. (1996) that
water curing as per the AASHTO specification [27]. A general trend of were empirically measured for a 102 mm � 205 mm cylinder [33,34,98,
increasing resistivity over time was observed, which is expected due to 99]. Although there was more variability at later ages, a similar trend to
continued hydration. The control mixture of 100% ordinary portland that presented in literature was observed [34,96,98]. The geometry
cement did not show significant increase beyond 28 days as the majority correction factor is approximately 1.9 for 102 mm � 205 mm cylinders
of hydration had occurred. Binary and ternary mixtures containing depending on exact dimensions and testing conditions [33,34,99]. The
SCMs had larger incremental increases in electrical resistivity at later regression analysis for this research study included nineteen concrete
ages, consistent with the pozzolanic reaction that occurs at later ages for mixtures with nine different SCMs, tested at multiple curing ages. The
many SCMs [1,40,96,97]. The rate of pozzolanic reaction is dependent strong correlation observed between surface and bulk resistivity in­
on several factors including the composition of the SCMs, replacement dicates that the relationship holds for various SCMs and remains
level, and temperature [1,46,79,96,97]; the pozzolanic reaction of SCMs consistent over time. The results were not noticeably affected by mixture
does not occur immediately because the cement must first hydrate design or SCM type.

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C.M. Tibbetts et al. Cement and Concrete Composites 107 (2020) 103491

Fig. 4. Correlation of measured surface and bulk resistivity of 19 concrete


mixtures at differing ages (7, 28, 56, 91, 182, and up to 365 days).

the control at 56 days were binary sugarcane bagasse ash mixtures. This
is in agreement with the surface and bulk resistivity results measured.
Surface and bulk resistivity test methods have been used as easier,
quick alternatives to the CIP test because of their strong correlation.
Bulk and surface resistivity results showed similar trends when
compared to the results from CIP testing as presented in Fig. 5; these
relationships are in good agreement with the literature [15,26,100,101].
Since these three test methods are based on electrical resistance and
have similar influencing factors, the results are expected to be strongly
related. A power curve was fitted to each of the data sets and the cor­
responding equations and R2 values are given in Fig. 5. The trend line of
theoretical bulk resistivity values calculated using Ohm’s law (Eq. (1)) is
also plotted for reference against the measured bulk resistivity values;
there is a slight divergence at lower CIP values (higher bulk resistivity
values), but the experimental values are still within the precision of the
ASTM C1202 test method [17] and there are fewer data points for that
range. The surface resistivity theoretical curve can be calculated by
multiplying the bulk resistivity by the geometry correction factor;
however, the limits given in AASHTO T 358 were the result of a large
experimental study and are slightly different than those calculated using
the geometry factor [15,27,34].

3.3. Water permeability vs. electrical test methods

Water permeability results show a general trend of decreasing

Fig. 3. Water permeability test setup.

3.2. Chloride ion penetrability

The CIP testing was performed in accordance with ASTM C1202 and
the results were calculated as the average charge passed for three
specimens and adjusted for the specimen diameter of 102 mm. CIP
testing was measured at curing ages 28, 56, 91, and up to 182 days, and
results ranged from approximately 6000 to 450 coulombs, spanning all
of the classifications in ASTM C1202 with the exception of “negligible”
[17]. All mixtures show a decrease in total charge passed over time
indicating a denser microstructure due to hydration; 7SF/50Slag,
20F/50Slag, and 10MK had the lowest charge passed, with a chloride
ion penetrability rating of “very low” at 56 days according to the rating Fig. 5. Correlation between CIP and surface resistivity (SR) and bulk resistivity
table in ASTM C1202 [17]. The only mixtures that did not outperform (BR) of 19 concrete mixtures at differing ages (28, 56, 91, and up to 182 days).

6
C.M. Tibbetts et al. Cement and Concrete Composites 107 (2020) 103491

permeability with time, with values ranging from approximately suggests that for these alternative SCMs, the water permeability test
1.5 x10-13 m/s to 1.2 x10-14 m/s. Water permeability testing was con­ method may be a better representation of the change in pore structure
ducted at ages 28, 56, 91, and up to 182 days of curing. As was seen with over time than the electrical resistivity test methods. Although the
the other test methods, the majority of mixtures had a lower water ground glass binary mixture was grouped with SCBAs, only two curing
permeability than the control mix for every testing age. The 20F and 20C ages (28 and 56 days) were evaluated for water permeability. The 20GG
mixtures had a high water permeability initially but a lower water mixture had better electrical resistivity than the control overall, but not
permeability than the control for the final ages; this is attributed to the as high as would be expected given the water permeability results.
slower pozzolanic reaction of fly ash and is consistent with other pub­ Since electrical resistivity results are known to be influenced by
lished literature [46,97]. factors other than the physical pore structure, the chemistry of the
The results from water permeability testing were then compared to sugarcane bagasse ashes and ground glass is likely the cause of the re­
the standardized electrical test methods to determine if relationships sistivity test overestimating the concrete penetrability. There is little
could be observed. Similar trends were observed for the comparison of research on the electrical resistivity or permeability of concrete con­
surface resistivity to water permeability and bulk resistivity to water taining SCBA; however, prior research has found that SCBA amended
permeability; based on the results from Fig. 4, the relationship between concrete tends to behave in a manner similar to traditional SCMs where
these test methods and water permeability was expected to be compa­ electrical resistivity increases and the total charge passed over the
rable. As a result, Fig. 6 includes only the surface resistivity data set as specimen decreases when compared to ordinary portland cement con­
there was slightly more variability than the bulk resistivity results. crete [76,89,96].
Overall the data showed increasing resistivity with decreasing water The initial linear relationship between water permeability and CIP
permeability, but there was an increase in variability once the water (ASTM C1202) for 61 data points was poor resulting in an R2 value of
permeability was below a threshold of approximately 6 x10-14 m/s. At 0.37 (dashed regression line in Fig. 7); however, after differentiating the
this point, the precision of the test method and sensitivity of flow mixture designs, trends based on SCM type were observed similar to
measurement begins to become too low to accurately measure the flow; those found in Fig. 6. The three sugarcane bagasse ashes (SCBA, SCBA-A,
an error in measurement of the specimen or reference cell of 1 mm for a and SCBA-B) were identified as outlying points from the behavior of the
24-hr time period gives an error in permeability of approximately other SCMs. Binary mixtures containing sugarcane bagasse ashes
1 x10-14 m/s. Therefore, the increased scatter for the low permeability exhibited higher total charge passed for CIP than other mixtures with
values and the minimum measured water permeability may be due to similar water permeability values; as a result, these mixtures were
the current limitations of the test method. omitted from the final linear regression (solid regression line in Fig. 7).
However, when isolating the mixture designs, different trends among The 20GG mixture also had a high CIP value compared to the general
the SCMs were discerned. Mixtures with traditional SCMs including fly trend and was removed from the final regression line. The resulting data
ash, silica fume, slag, and metakaolin had similar behavior, as set of 40 points, representing traditional SCMs, shows increasing total
decreasing permeability is related to increasing resistivity which is charge passed over the specimen with increasing water permeability and
plotted in Fig. 6a; ternary mixtures including 20C/10SCBA and has a higher R2 value of 0.71. The relationship observed is expected as
20C/5GG are also included in Fig. 6a. The alternative SCMs (binary higher water permeability would indicate higher interconnected
mixtures of SCBA, SCBA-A, SCBA-B, and ground glass) mixtures per­ porosity and thus more electrical current should be able to pass through
formed similarly to each other; in contrast to the traditional SCMs, the the specimen. The ternary mixtures (20C/10SCBA and 20C/5GG) fol­
electrical resistivity values were lower and did not show much increase lowed the general trend of the traditional SCMs and were not removed
with age, while the water permeability values showed larger changes from the regression due to the low inclusion rate of SCBA and GG.
over time as shown in Fig. 6b. The 20GG 56-day point had the highest The thresholds for the chloride ion penetrability classifications as
surface resistivity of the alternative SCMs in Fig. 6b with 18 kΩ-cm, given in ASTM C1202 were marked in Fig. 7 as horizontal dotted lines
while the majority of the alternative SCM mixtures classified as “high” [17]. Equivalent classification threshold values were developed from the
chloride ion penetrability (<12 kΩ-cm) across all testing ages. regression line of the water permeability testing results (excluding GG
Conversely, the water permeability results for the alternative SCMs and SCBA binary mixtures), and are shown as vertical dotted lines in
showed almost an order of magnitude difference between the highest Fig. 7. The resultant equivalent ranges for chloride ion penetrability
permeability of 1.1 x10-13 m/s and the lowest value of 3 x10-14 m/s. This based on water permeability are provided in Table 3. The classification

Fig. 6. Comparison of water permeability and surface resistivity results from differing ages, with each data point representing the average of three specimens.

7
C.M. Tibbetts et al. Cement and Concrete Composites 107 (2020) 103491

majority of mixtures also either remained the same or decreased at 56


days. The pH and conductivity of the pore solution are directly related
and expected to decrease with time as calcium hydroxide is consumed by
the pozzolanic reaction that occurs with supplementary cementitious
materials; lower pH and conductivity values indicate relatively high
pozzolanic activity [1,40,87,102].
For the majority of the mixtures, a reduced pore solution conduc­
tivity generally trended well with higher surface and bulk resistivity and
reduced CIP charge passed. However, the electrical conductivity of bulk
concrete can be described by a combination of the total volume of
interconnected pore fluid, the conductivity of the pore fluid, and the
conductivity of the bulk solids. Minor fluctuations in pore fluid con­
ductivity will likely not dictate systematic electrical behavior.
The mixtures that had the highest conductivity (and pH) values were
those containing ground glass while the mixtures with the lowest con­
ductivity (and pH) contained silica fume. The low alkali content and fast
Fig. 7. Relationship between water permeability and CIP for 19 concrete pozzolanic reaction of silica fume results in a low conductivity. This is
mixtures. The dashed regression line includes all mixtures and the solid supported by literature that has shown silica fume to be highly reactive
regression line includes traditional SCMs, but excludes SCBA, SCBA-A, SCBA-B, and efficient at reducing the pore solution alkalinity [1,40,97].
and 20GG. Chloride ion penetrability classification thresholds from ASTM Ground glass can have variable chemical composition and reactivity
C1202 are shown as dotted lines. based on the glass source and processing; the relatively low surface and
bulk resistivity (and high total charge passed) observed is assumed to be
of chloride ion penetrability based on water permeability is in general due to the high alkali content of the ground glass in this study
agreement with the classifications based upon CIP testing. From this (approximately 13% Na2Oeq) and resulting high pore solution conduc­
data set, water permeability above 1.3 x10-13 m/s is classified as high tivity (65–79 mS/cm) [39].
penetrability, 3.2 to 6.4 x10-14 m/s is low, and values with an order of The binary sugarcane bagasse ash mixtures had the lowest surface
magnitude of x10-15 m/s are considered very low to negligible. and bulk resistivity (and highest total charge passed) of the SCM types
The slope of the final regression line was not appreciably affected by investigated; however, the conductivity of the pore solution was rela­
curing age. As the specimens matured and the water permeability results tively low. The low pH and conductivity of pore solution indicates
were classified as low or very low, the R2 value decreased. This increased reduction of alkali hydroxides due to pozzolanic activity and could also
scatter is attributed to the smaller range of water permeability values be influenced by the relatively high phosphorus (P2O5) levels due to the
and the reduced accuracy of the flow measurements for the low acidic and less conductive nature of P2O5 [103]. The low conductivity of
permeability ranges. All of the concrete mixtures evaluated in this the pore solution combined with electrical testing results suggests that
research study were mixtures with a w/cm of 0.37; typical concrete either the pore structure is not as refined (more pathways for flow), or
produced has a higher w/cm and would be expected to have higher the bulk concrete matrix is more conductive due to presence of electri­
water permeability, resulting in less scatter and more accurate cally conductive constituents. As water permeability measures the
classification. physical pore structure, the results show that the pore matrix of the
From the results of the electrical test methods, it was anticipated that SCBA mixtures is refined; therefore, it is concluded that the composition
the mixes containing GG and SCBA would perform poorly in water of the SCBA mixtures are composed of electrically conductive bulk
permeability testing. When these results were contradictory to expec­ material (rather than pore fluid).
tations, an investigation into the potential causes for this discrepancy The SCBA used in this research had high LOI values ranging from 12
was conducted. As electrical testing methods can be affected by pore to 42%; whereas SCBA material in literature had values ranging from 3
solution irrespective of actual physical pore structure [1,33], the pore to 6% [76,89]. The LOI values for SCBA, SCBA-A, and SCBA-B were 42%,
solution of the mixes was analyzed to determine if pH or conductivity 24%, and 12%, respectively (Table 2). For SCBA and other agricultural
provided a potential explanation for the contradictory results. wastes, material processing to obtain a homogeneous material can be
challenging and variability is typically high. The majority of research on

3.4. Pore solution analysis


Table 4
Pore solution was expressed from cementitious paste specimens at 28 Pore solution pH and conductivity results for cementitious paste specimens at
and 56 days for pH and conductivity (millisiemens per centimeter) 28-day.
analysis to evaluate the influences of the SCMs on pore solution char­ Mixture pH Conductivity (mS/cm)
acteristics; the results of 28-day testing are presented in Table 4. The pH OPC – Control 13.2 52.1
values ranged from 12.7 to 13.3 and either remained the same or 20F 13.3 49.5
decreased slightly at 56 days. Conductivity measurements for the 20C 13.3 66.7
7SF 12.7 13.3
50Slag 13.1 37.2
Table 3 20F/50Slag 13.0 26.8
Equivalent empirical water permeability thresholds based on chloride ion 10MK 13.1 31.9
penetrability classifications from ASTM C1202. 10SCBA 13.1 37.1
20C/10SCBA 13.1 40.4
Chloride ion ASTM C1202 charge Equivalent empirical water
7SF/50Slag 12.7 10.7
penetrability passed (coulombs) permeability (x10-15 m/s)
20C/50Slag 13.0 28.9
High >4000 >130 30C/5F 13.3 59.3
Moderate 2000–4000 64–130 20GG 13.3 72.4
Low 1000–2000 32–64 20C/5GG 13.3 64.7
Very low 100–1000 3.2–32 20SCBAa 12.9 21.4
Negligible <100 <3.2 a
This cementitious paste mixture had a w/cm of 0.5 for workability.

8
C.M. Tibbetts et al. Cement and Concrete Composites 107 (2020) 103491

SCBA for use in concrete has focused on the calcination and grinding of classifications for qualifying concrete durability.
the material to achieve optimum pozzolanic activity [76–78,83–89].
The high LOI in SCBA is attributed to elevated levels of unburnt carbon Disclaimer
in the material [78,84,89]. Thermal carbon blacks are known to have
conductivity in the range of 0.1–100 S/cm [104,105]; this conductivity The views and opinions presented in this document may not repre­
is a potential explanation for the conductive nature of the bulk matrix sent the official views of the State of Florida, the Florida Department of
for SCBA mixtures. Unburnt carbon in agricultural waste ashes can be Transportation or the University of Florida.
reduced by using higher calcination/boiler temperatures to reduce the
carbon content [78,84,89]. Acknowledgements

4. Conclusions The authors acknowledge the support received from the Florida
Department of Transportation for funding this research, contract num­
This research investigated the relationships between standardized ber BDV31-TWO-977-42. The authors would also like to express their
electrical test methods (ASTM C1202, AASHTO T 358, and AASHTO TP gratitude to the following people at the FDOT SMO; Dr. H.D. DeFord for
119) and pressurized uniaxial water permeability to evaluate the accu­ his valuable advice, and Ronald Simmons and Teresa Risher for their
racy of using electrical measurements as a tool for predicting concrete assistance with testing. The authors would also like to acknowledge the
penetrability. Nine different supplementary cementitious materials were following personnel from the University of Florida, Dr. Taylor
evaluated as part of this study, and differences in behavior between Rawlinson, Taylor Humbarger, Paul Schwartz, Neal Turner, Jason
traditional and alternative SCMs were observed. Subsequent to contra­ McAllister-Pringle, Margaret Long, Jeanine Marrou, and Alexander
dictory results between electrical and water permeability testing Campano.
methods, the pore solution from cementitious paste specimens was
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