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CHAPTER THREE

EXPERIMENTAL WORK

3.1 General
The experimental work dealt with the preparation and testing of
constituents of concrete mixes according to standard specifications to produce
high quality concrete having corrosion resistance in aggressive solutions.
However, physical tests included: compressive strength, water absorption and
electrical resistance tests were employed. The investigation of corrosion problem
of embedded steel in concrete in term of time to corrosion initiation was
conducted using half-cell potential system, while accelerated corrosion technique
was used to measure corrosion current with time to cracking of concrete cover
due to reinforcement steel corrosion in chloride solution and chloride-sulfate
containing solution. The effect of water reducing agent admixture (HRWRA
additive) on the reinforcement corrosion was also studied and evaluated. The
details of experimental work, properties and specifications of materials, mix
proportions and concrete tests are presented in this chapter. Figure (3.1)
illustrates the details of the experimental program adopted throughout the present
study.

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Chapter Three

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3.2 Experimental Work


The experimental included the description of the: a) materials, b)
solutions, and c) reinforcement.

a) Materials
Cement
sulfate Portland cement, type V, ASTM C 150 [56], commercially known
(valkon), produced in Pakstan was used in the present study. The chemical
composition and physical properties testing were carried out in the "Laboratory
of Civil-Engineering Department-College of Engineering-University of Basra".
The results indicated that the cement conformed to Iraqi specifications No.
5/1984 [57], appendix (A) Tables (A1 and A2).
Fine Aggregate
Natural sand from Al-Zubair, Basra south region was used. The sulfate
and chloride content and sieve analysis of the fine aggregate used are illustrated
in appendix (A) Tables (A3 and A4), respectively. These conformed to Iraqi
specifications No.45/1984 [58].
Coarse Aggregate
Crushed gravel of 19mm maximum size was used as coarse aggregate.
The sulfate and chloride content and sieve analysis results of the coarse
aggregate are illustrated in appendix (A) Tables (A3 and A5), respectively.
These conformed to Iraqi specifications No.45/1984 [58].
High Range Water Reducing Admixture (HRWRA)
High range water reducing admixture (HRWRA) superplasticizer, sold
commercially as (plastocrete-N) was used. It is a chemical base of Modified
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Chapter Three

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Lignosulphonate. It acts both as a highly efficient plasticizer and water proofing


agent complies with ASTM C 494 Type F [59]. The properties of this admixture
(as claimed by the producer: Sika Company) are presented in appendix (B).
Water
Ordinary desalinated water of total dissolved solids < 100 mg/l was used
without any additives for mixing and curing of concrete.
b) Solutions
The solutions used in the present study are:
1) 3.5% sodium chloride (NaCl) solution was prepared by dissolving 35 g
commercial NaCl (purity 90% w/w) in one liter distilled water.

2) 5% sodium sulfate (Na2SO4) solution was prepared by dissolving 50 g


Na2SO4 (purity of 99 %, BDH chemical company) in one liter distilled
water.

c) Reinforcement Steel
For corrosion testing measurements, deformed steel bars of 12 mm
diameter and 200 mm length were used for the test of reinforcement specimens.
The chemical composition (wt %) was carried out using "Spectrometric
Analytical Instrument" (TXC25 model, 1200137, Germany), in the applied
mechanics laboratory-Department of Mechanical Engineering-College of
Engineering-University of Basra. The results were shown in Table 3.1. Three
tensile bars specimens were tested in "the Laboratory of Manufacturing Process
Materials Engineering Department-College of Engineering-University of Basra".
The testing results for deformed bars (grade 40) were compared to the ASTM
A615/A615M-04b [60]. The results of testing of the properties of reinforcing
bars are presented in Table 3.2. All bars were treated according to the procedure
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Chapter Three

Experimental Work

given by ASTM G1-03 [61] by pickling with a 10% sulfuric acid (H 2SO4)
solution for 5 minutes, and then rinsed in water prior to wire brushing to remove
any remaining rust. The bars were wipped with clean cloth and allowed to airdrying. Then un-embedded end of the bar was coated with chemical resistance
epoxy paint (See appendix-C) then covered by electroplater's tape in order to
eliminate the crevice corrosion , leaving an inside 112.5 mm length of bar
uncovered.
Table 3.1 Chemical composition (wt %) of the used steel.
Fe

Si

Mn

Cr

Mo

98.500

0.200

0.080

0.900

0.005

0.005

0.085

0.003

Ni

Al

Co

Cu

Nb

Ti

0.025

0.010

0.010

0.028

0.003

0.003

0.003

0.025

Table 3.2 The results of testing of physical properties of deformed steel bars.

Properties

Test results

Yield

Ultimate

Elongation

strength

strength

(MPa)

(MPa)

400

572

16

280

420

12

ASTMA615/615M-04b
minimum. Limit

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Chapter Three

Experimental Work

3.3 Measuring Devices


1. Spectrometric Analytical Instrument (TXC25 model, 12001137, Germany)
shown in Figure (3.2) was used for determination of chemical composition of
reinforcement steel.
2. Electronic precision balance; two decimal, (max. capacity 600 g) as shown in
Figure (3.3).
3. Compressive machine (Model C070PD161, Italy) shown in Figure (3.4), used
for measuring the compressive strength of concrete specimens.
4. DC power supply, Type" TU-305D" used for accelerated corrosion test.
5. Digital multimeter, Fuke, model "DT 9205" used for corrosion test.
6. Saturated calomel as reference electrode (SCE), Karl-Kolb, Figure (3.5).
7. Electrical furnace, Type "Thermolyne", _UK, temp. range (0-1050 C).

3.4 Concrete Mix Specifications


Concrete mixes were designed according to the absolute volume method,
and proportioning of materials was carried out on weight basis. A concrete mix
3

with cement content of 405 kg/m , while the effective water to cement ratio of
0.45. The mixing ratio 1: 1.5: 3 for cement, sand, and gravel respectively were
utilized in all the concrete mixtures. The materials were mixed by an electrically
driven batch mixer.
Six types of concrete mixes were prepared throughout the present study:
1. One concrete mix: this was prepared as reference concrete mix without any
admixture.
2. Four concrete mixes: containing super plasticizer in four percentages (0.125%,
0.250%, 0.375%, and 0.500% by weight of cement).

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Chapter Three

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3.5 Determination of the concrete workability and water reduction


The workability of all concrete mixes was measured using the slump test
in accordance with the procedure described in BS.1881: part 2 [62]. The
water/cement ratio for all mixes are adjusted to maintain equal workabilities of
100 5 mm. At each dosage of high range water reducing admixture (HRWRA),
the water/cement ratio was adjusted for a given slump and evaluating the
corresponding water reduction at each stage by the following equation [62]:
w
w
reference
test mix
c
% = c
100
w
c reference

(3.1)

The water reduction reached its maximum value at the optimum dosage of
HRWRA. Table 3.3 shows the water reduction for various types of concretes
relative to reference concrete.

3.6 Preparation and Casting of the Test Specimens


A total number of (130) specimens were prepared with the specified
dimensions and geometrical shapes of reinforced concrete as illustrated in Table
3.4. For normal concrete and HRWRA-containing concrete, the following
procedures were performed according to the method given in BS 1881: parts108
[63] and 110:1983 [64], which can be summarized as follows:
1. The dry constituents of mix were initially mixed for 1.5 minutes using a rotary
mixer.
2. The required dosage of admixture HRWRA was added to half amount of
required water and followed by one-minute mixing.

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Chapter Three

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3. The remaining quantity of water was added and the mixture was mixed for
further two minutes and the water was adjusted to maintain a slump within the
range of 100 5 mm for each mix.
4. The molds were cleaned and oiled before casting and compacting then the
specimens were covered with polyethylene sheets to prevent moisture
evaporation from the concrete surface.
Table 3.3 The proportions of HRWRA admixture for each mix and w/c
reduction calculated from equation 3.1.
Type of mixes
Reduction in W/C
Symbol of mix

HRWRA %

W/C

ratio

Ratio

Ref.

0.000

0.45

0.000

MS1

0.125

0.43

4.445

MS2

0.250

0.42

6.667

MS3

0.375

0.40

11.111

MS4

0.500

0.37

17.780

3.7 Curing of the Test Specimens


The test specimens were taken out from the molds after 24 hours of
casting and completely immersed in desalinated water. Then, the cubical
specimens were immersed in chloride and chloride-sulfate solutions for periods
of 3, 7, 28, 60, and 90 days for concrete testing. While, the reinforcement
cylindrical specimens partially immersed in corrosive solutions mentioned above
for corrosion tests.
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Chapter Three

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Table 3.4 Details of the test specimens.


Number of Samples

Dimensions-mm

Type of Test
Performed

50 samples (150 Cube)

100x100

Compressive Strength

20 samples (60 Cube)

100x100

Water Absorption

40 samples (120 Cube)

100x100

Electrical resistance

75x150

Electrochemical Tests

20 Cylinder

3.8 Concrete Tests


The test of concrete included compressive strength, absorption after
immersion and electrical resistance.

3.8.1 Compressive Strength Test


The compressive strength test was carried out for three replicate
specimens according to BS 1881, part 116:1989 [65]. Cubes with dimensions of
(100x100x100) mm were tested using a 2000 kN capacity compression machine
provided with a digital indicator as shown in Figure (3.4). The tests were
performed at ages of 3, 7, 28, 60, and 90 days.

3.8.2 Absorption after Immersion


The most important characteristic of concrete in resisting aggressive
species ingress is its permeability. To illustrate the effect of adding different
percentages of chemical admixture on cement absorption ability of hardened
concrete, three cubic specimens (100x100x100 mm) were cast and left embedded
into a solution in humid atmosphere for 28 and 90 days then dried in an oven at a
temperature of 100 to 110C for 24 h. After removing each specimen from the

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Chapter Three

Experimental Work

oven, it was allowed to cool in dry air to a temperature of 20 to 25C and the
mass (A) was determined. The specimens were immersed again in solution for
48 h. It was surface-dried, by removing surface moisture with a moistened towel,
and its mass (B) was re-determined according to ASTM C 642-97. The
absorption after immersion can be determined according to following equation
[66]:

= (

) 100

(3.2)

A = mass of oven-dried sample in air, g


B = mass of surface-dry sample in air after immersion, g.

3.8.3 Electrical Resistivity Test


Direct current (D.C) measurements were carried out on 100 mm cube
throughout the present investigation. A constant electric field was applied
between two electrodes and the resulting current was measured. The circuit used
was arranged as shown in Figures (3.6 and 3.7) for external plate electrodes.

Test Procedure
The D.C. electrical resistance measurements was carried out using a)
Power supply and b) two multimeters, for voltage and current measurements and
can be explained as follows:
1. The gap between the test specimens and the external brass plate
electrodes was filled by cement paste with w/c ratio equal to that of
specimen tested itself , to avoid a significant change in resistivity.
2. The instruments are turned

on , and

the

high

performance

digital

multimeter which was used as a voltage measuring device was set on


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Chapter Three

Experimental Work

D.C. voltage mode. While, the second digital multimeter was set on D.C. current
mode.
3. The specimens response to each voltage unity from 1-10 volts was recorded.
At every selected voltage, the simultaneous values of current were recorded. The
resistance of concrete was determined by the reverse slope of the line of voltagecurrent plot.

3.9 Corrosion Monitoring Techniques


The corrosion of steel embedded in concrete is not visually evident until
the damage reaches the external signs of deterioration such as rust spots, cracks
or spalling. It is necessary to use non-destructive techniques for assessing the
corrosion activity and measuring the corrosion rate of reinforcement. The
corrosion monitoring of steel in concrete such as half-cell potential measuring
circuit was adapted and explained in the following text.

3.9.1 Half-cell potential Measurements


The half-cell potential as an electrochemical potential system was
employed including reinforcing steel as working electrode. The potential was
measured with respect to reference electrode i.e. saturated calomel electrode
(SCE). The measurements were carried out according to the method given by
ASTM C876-80 standard [67].

A) Test specimens
The concrete cylinders of 75x150 mm reinforced with central deformed
bar of 12 mm diameter were used as illustrated in Figure (3.8). The working
electrode is presented by 1 m long an isolated copper wire welded to the upper
portion of reinforcement bars thats exposed to air.

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Chapter Three

Experimental Work

B) Test procedure
The half-cell potential measurements were carried out using a) reference
electrode-SCE and b) high performance digital voltmeter, as D.C. potential
measuring instrument and can be explained as follows:
1. The reinforcing steel is electrically connected to the positive terminal of
voltmeter and the reference electrode to the negative terminal of the same
voltmeter, Figure (3.9).
2. The reference electrode was placed adjacent to the working electrode of the
test specimen and only the porous end immersed in the solution, Figure (3.10).
3. The function switch of the voltmeter is turned to D.C , and the range
switch to 2 volt range, then the half-cell potential can be read directly on the
display of voltmeter. The results of half cell potentials can be interpreted
according to ASTM C876 [67] as in T able 3.5. The results obtained were shown
in the chapter of results and discussion.
Table 3.5 Corrosion interpretations (ASTM C876) [67].
Half-cell potential reading,

Corrosion activity

mV SCE
< -400

Severe corrosion

< -270

High risk of corrosion (90%)

-120 to -270

uncertain corrosion risk

> -120

Low risk of corrosion (10%)

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Chapter Three

Experimental Work

3.9.2 Accelerated Corrosion and Current Measurements System


A cylindrical concrete specimen 75 mm in diameter and 150 mm height
with embedded steel bars were cast. Epoxy paint was applied to the unembedded end of the bar and at the interface of concrete and air to avoid the
initiation of corrosion at those critical locations. These specimens were then
subjected to an accelerated corrosion test to determine the susceptibility of
reinforcing steel to corrosion [68].
The accelerated corrosion setup used in the present study consisted of
plastic tank (600 mm length, 500 mm width and 400 mm depth) filled with
electrolytic solution (aggressive solutions 3.5% sodium chloride and 5% sodium
sulfate) and steel mesh placed at the bottom of the tank. The concrete cylinders
were then placed in a tank. Each cylinder was partially immersed in the
electrolyte up to two-thirds of its total height. To eliminate any variation in the
concentration of the salts and pH of the electrolytic solution, it was renewed on a
weekly basis. The specimens steel bars and the bottom steel mesh in the tank
was connected to a 12 V DC power supply. The direction of the current was
arranged so that the steel mesh served as a cathode while the specimen bars
served as anodes, Figure (3.11). After the power supply was turned on, the
current flowing through the system was recorded at one-hour intervals. The
current supplied to each of the specimens was plotted against time and the time
current curves were utilized to evaluate the time to cracking of concrete due to
reinforcement corrosion [69].

3.10 Measurements of mass Loss


After the reinforced concrete specimens were corroded and the
measurements of half cell and current values were taken, the concrete were jack

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Chapter Three

Experimental Work

hummered to remove the corroded bars. The corroded bars were cleaned with a
wire brush to ensure they were free of any adhering concrete or corrosion
products, and then soaked in a chemical solution (1:1 of HCl and water)
according to ASTM G1-03 method [61]. The clean bars were then reweighed and
the percentage mass loss for each bar was calculated based on equation (3.4)

% =


100

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(3.4)

Chapter Three

Experimental Work

Preparation of Materials

Mixing

Fresh Concrete

Casting into Cubic and


Cylindrical Specimens

Slump Test

Curing

Testing

Concrete Testing
Testing

Electrochemical Measurements

Half-cell
Potential
Measurement
s

Compressive
Strength Test
Absorption
Test

Accelerated
Corrosion
Measurement
s
Weight Loss

Electrical
Resistance
Test

Evaluation of Testing Results


Test results
Fig. (3.1) Details of The Experimental Program.

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