Construction and Building Materials 38 (2013) 1058–1065

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Construction and Building Materials

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Evaluation of fly ash and Metakaolin concrete at elevated temperatures

through stiffness damage test
Abid Nadeem a, Shazim Ali Memon b,⇑, Tommy Yiu Lo b
a
Department of Civil and Architectural Engineering, Qatar University, Doha, Qatar
b
Department of Civil and Architectural Engineering, City University of Hong Kong, Hong Kong

h i g h l i g h t s

" HPC was evaluated at elevated temperature through Stiffness Damage Test (SDT).
" The stiffness and elasticity decreased while damage increased with the increase in temperature.
" For all mixes, significant change in the SDT parameters occurred at 300 °C.
" Plastic strain and damage index correlate well with loading elastic modulus.

a r t i c l e i n f o a b s t r a c t

Article history: This research work was carried out to evaluate the performance of High Performance Concrete (HPC)
Received 23 May 2012 made with Fly Ash (FA) and Metakaolin (MK) at elevated temperature through Stiffness Damage Test
Received in revised form 22 August 2012 (SDT). Variables of the test program include partial replacement of cement with MK (10% and 20%)
Accepted 21 September 2012
and FA (20% and 40%) and temperature from 27 to 400 °C. To quantify the damage, chord loading mod-
Available online 3 November 2012
ulus, unloading stiffness, plastic strain, damage index and non-linearity index were evaluated from SDT.
Correlation among SDT parameters and in between SDT parameters and elevated temperature were also
Keywords:
studied.
Elevated temperature
Fly ash
According to the test results, the SDT parameters showed that the stiffness and elasticity decreased and
Metakaolin damage increased with the increase in temperature. The stiffness changes were evident from chord mod-
Modulus of elasticity ulus and unloading stiffness, elasticity changes from plastic strain and damage to concrete from damage
Damage index index. For all mixes, significant change in the SDT parameters occurred at 300 °C. Therefore, 300 °C can be
Plastic strain considered as critical temperature. At elevated temperatures (300 °C and 400 °C), FA mixes showed lower
values of plastic strain and damage index than MK mixes. Thus, it may feasible to increase the allowable
working temperature for FA mixes. The SDT parameters were found to be sensitive to elevated temper-
atures caused by changes in the microstructure of concrete. Test results also revealed that plastic strain
and damage index correlate well with loading elastic modulus with values of coefficient of correlation
equal to 0.9657 and 0.9835 respectively. Therefore, plastic strain and damage index measured from
SDT can be used to estimate the percentage residual chord loading modulus of concrete affected by fire.
Strong correlation also exists between PS and DI with coefficient of correlation equal to 0.985.
Ó 2012 Elsevier Ltd. All rights reserved.

1. Introduction
Fire remains one of the serious potential risks to most of the
buildings and structures [1]. The extensive use of concrete as a
structural material has led to the demand to fully understand the
effect of fire on concrete. Due to composite nature of concrete
and different thermal characteristics of constituents, its perfor-
⇑ Corresponding author.
E-mail addresses: abid@qu.edu.qa (A. Nadeem), shazimalimemon@gmail.com
(S.A. Memon).
mance is greatly affected by high temperature [2,3]. The issues re-
lated to the exposure of concrete to the elevated temperatures
pose concerns about the serviceability and stability of the structure
which, in turn, are related to human safety. Also, after a fire inci-
dent, one of the prime concerns is to determine the residual prop-
erties so as to assess the load bearing capacity of structures.
The inclusion of eco-friendly materials in HPC to improve the
mechanical and durability properties may require the assessment
of its fire resistance capabilities [4,5]. Many researchers have as-
sessed the mechanical and durability performance of fly ash con-
crete [6–9] at elevated temperatures. It was found that the FA

0950-0618/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.conbuildmat.2012.09.034
 A. Nadeem et al. / Construction and Building Materials 38 (2013) 1058–1065 1059

improved the performance of concrete at elevated temperatures Table 1

and this improvement was more significant at temperatures below Composition of OPC, FA and MK.

600 °C [10]. Poon et al. carried out the investigation into perfor- OPC FA MK
mance of Metakaolin at elevated temperatures [11]. They found Chemical composition (%)
that concrete with higher replacement of MK (20%) suffered higher Silicon dioxide (SiO2) 19.6 56.8 53.2
loss in strength at all temperatures and suggested that severe dura- Aluminum oxide (Al2O3) 7.3 28.2 43.9
bility loss occur at elevated temperatures. Ferric oxide (Fe2O3) 3.3 5.3 0.38
Calcium oxide (CaO) 63.1 3.0 0.02
High Strength Concrete (HSC) is considered more brittle than Magnesium oxide (MgO) 2.5 5.2 0.05
normal strength concrete (NSC) and is investigated to have more Sodium oxide (Na2O) 0.1 – 0.17
linear elastic behaviour with E-modulus higher than NSC [12]. Potassium oxide (K2O) 1.1 – 0.10
For unstressed tests there is no significant difference in the modu- Sulfur trioxide (SO3) 2.1 0.7 –
Loss on ignition 3.0 3.9 –
lus of elasticity–temperature relationship of HSC and NSC [13]. A
temperature of 300 °C marks the beginning of higher rate of de- Physical properties
Specific gravity 3.16 2.31 2.62
crease in modulus of elasticity in HSC [1]. The pattern of loss in
Specific surface (m2/kg) 312 412 12680
E-modulus values is more or less the same as in NSC [14]. Unlike Initial setting time (Min) 125
normal strength concrete, Young’s Modulus of HSC is also affected Final setting time (Min) 240
by the elastic properties of aggregates [15].
Cyclic loading investigations are necessary for improving the
high-cycle fatigue (e.g. service loading of bridges) and low-cycle fa- 2.3. Curing details
tigue (e.g. earthquakes) of concrete. Cyclic loading accelerated the
shifting and enhanced the micro-cracking process. These cracks For curing, the specimens were removed from the moulds after 24 h of casting
would develop gradually. The higher the stress levels and the and placed in water tank at 27 °C for 28 days and then in a humidity (65%) and tem-
perature (27 °C) controlled room for further five months.
greater the stress ranges, the higher the supplied energy and the
more rapid the cracks developed. For HSC, it had a steeper stress
strain curve as compare to the NSC [16,17]. 2.4. Heating and cooling details
The cyclic loading of concrete after subjecting to high tempera-
The concrete specimens were heated to elevated temperatures (200 °C, 300 °C
tures was investigated by Nassif [18,19]. The author introduced a
and 400 °C) at the age of about 180 days using automatic electric furnace. The fur-
new classification system for fire damaged concrete based on the nace had the rating of 1280 °C with programmable microprocessor temperature
strain energy dissipated in a hysteresis loop. They defined chord controller attached to the furnace power supply and equipped with thermocouples
loading modulus, unloading stiffness, damage index, plastic strain for furnace temperature measurement. The specimen temperatures were also mea-
and non-linearity index based on SDT. These five parameters were sured with thermocouple embedded at the centre of the sample. Furnace had the
ability to provide heat from two sides and the bottom. The specimens were heated
used as the basis to classify, quantify and compare the damage that
to ensure the steady state [20]. Accordingly, the test specimens were placed in the
occurred at elevated temperature. furnace starting from normal temperature and heated at a rate of 5 °C/min up to the
The fire resistance of concrete is highly dependent on its con- peak furnace temperature. The peak temperature was kept constant up to the time
stituent’s materials, particularly pozzolans [11]. Therefore, it is when steady state was established. It was observed that the time from the start to
the setting up of steady state ranged from 3 to 4 h for all the specimens.
necessary to have a complete knowledge of pozzolanic concretes
For cooling, the furnace was switched off after reaching the steady state and the
which are extensively used in oil, gas, nuclear and power indus- specimens were allowed to cool in the furnace overnight with the door of the fur-
tries. So far no experimental data is available regarding chord load- nace open for easy dissipation of heat and tested after 24 h.
ing modulus, unloading stiffness, damage index, plastic strain and
non-linearity index for concrete made with fly ash and especially
2.5. Details of SEM test
with Metakaolin subjected to elevated temperatures.
In this research, five HPC mixes made with FA and MK were The concrete cubes (100 mm) were cut into two or three slices of 12 mm thick-
investigated. Variables of the test program include partial replace- ness using rotary saw. The outer 5 mm strip was discarded because of a likely infe-
ment of cement with MK (10% and 20%) and FA (20% and 40%) and rior hydration due to escape of moisture by evaporation. From 12 mm thick slice, a
temperature from 27 to 400 °C. To quantify the damage, chord strip of 12 mm  12 mm cross section and 100 mm length was cut. The cutting pro-
cedure has been schematically shown in Fig. 1. The middle strip was then cut at
loading modulus, unloading stiffness, plastic strain, damage index about 30 mm from one of the end using rotary saw. Fractured specimens were pre-
and non-linearity index were evaluated from SDT. Correlation pared from concrete specimens. The position of fracture at a specific place along the
among SDT parameters and in between SDT parameters and ele- length of strip was selected where the fractured surface could comprise a neat
vated temperature were also studied. interface of paste and aggregate. A V-groove was made at the selected position as
a crack-inducer for fracture. The prism was clamped and then fractured by a firm
2. Experimental investigation knock. Fig. 2 shows the process schematically. The fractured surface was then cut
away from the strip in a slice of not more than 5 mm thickness by using a precision
2.1. Materials diamond saw. The thin fractured slices were immersed in acetone to stop further
hydration in the surface zone and cleaned from free particles produced during spec-
Ordinary Portland cement (OPC), low-calcium pulverised fuel ash and Metaka- imen cutting and fracture operations in an ultrasonic vibrator. The specimens were
olin were used for making HPC mixes. The chemical composition and physical prop- then stored in clean acetone until heating in the furnace. Heating of SEM specimens
erties of these materials are given in Table 1. in furnace was performed at a heating rate of 1 °C/min up to the desired tempera-
River sand and crushed granite were used as fine and coarse aggregates. The tures. The low heating rate minimized high temperature gradients in the specimens
particles of fine aggregates had the specific gravity of 2.61, 24 h absorption value and thus differential thermal cracking in specimen was avoided. The specimens
of 0.7% and fineness modulus of 2.4 while coarse aggregate particles had specific were then further treated for preparations normally performed for SEM which in-
gravity of 2.62 and 24 h water absorption 0.6%. A sulphonated naphthalene formal- clude vacuum drying and gold coating.
dehyde condensate was used in adequate quantities in the mixes to achieve desired
slump of 100 mm and above.
2.2. Mix proportions 2.6. Stiffness damage test

Five HPC mixes including one control mixe (PC) mix, two metakaolin mixes and
two fly ash mixes were investigated. Metakaolin was used in replacement level of
10% and 20% (MK10 and MK20) while fly ash was introduced in replacement level
of 20% and 40% (FA20 and FA40). The details of mix along with 28 days compressive
strength determined by BS 1881: Part 116 1983 are given in Table 2.
The SDT was conducted in a 1600 kN Rock Mechanics Test System using the
50kN range in load control mode. The cylinder specimens were fitted in compress-
ometer rings, which comprise two reference rings each clamped to the specimen
100 mm apart by three hardened stainless steel pins spaced equally around the cir-
cumference. The compressometer was fitted at mid-height of the specimen in order
1060 A. Nadeem et al. / Construction and Building Materials 38 (2013) 1058–1065

Table 2
Mix details of HPC (per m3).

Mix 28 days Compressive Cement (kg) FA (kg) MK (kg) Water (kg) Sand (kg) Aggregate (kg)
strength (MPa)
20 mm 10 mm
PC 85.7 450 0 0 135 643 797 399
MK10 105.8 405 0 45 135 641 794 397
MK20 111.3 360 0 90 135 638 791 395
FA20 98.8 360 90 0 135 634 786 393
FA40 86.6 270 180 0 135 625 774 387

Fig. 1. Specimen preparation for SEM test.

Fig. 2. Fractured specimen making process.

to avoid the end effects of the platens when monitoring strain within the uniaxial
stress field. The axial displacement was measured by two similar linear variable dif-
ferential transducers mounted vertically at 180° intervals around the specimen.
The loading machine was controlled by a computer programme, loading to a
maximum compression stress of 6.366 N/mm2 at a constant rate of 800 N/s and
then reduced to 0.637 N/mm2 at the same rate. The maximum stress level of
6.366 N/mm2 was adopted to keep the applied stresses on the specimen in elastic
range. This loading and unloading cycle was performed five times before fully
unloading the specimen. The test data from the load/displacement transducers
were logged every second by Data Logger TDS-303. Output from Data Logger was
via RS 232 interface to a personal computer and calculations were performed with
the help of spreadsheet programme.
The peak temperatures adopted were 200 °C, 300 °C and 400 °C. The tempera-
tures higher than 400 °C were not selected as the existing knowledge [18,19] pro-
vides that at temperatures above 400 °C the stiffness suffers severe damages and
hence the temperatures above 400 °C were not investigated in the research.
The five parameters calculated in SDT have been defined in Fig. 3 [18]. Chord
modulus (Ec) is the slope of the chord of loading curve. Unloading stiffness (Eu) is
the slope of the chord of unloading curve. Ec and Eu are measured in GPa (Giga Pas- Fig. 3. Definition of SDT parameters (Adopted from [19]).
cal). Plastic strain (PS) is the un-recovered strain after unloading. Plastic strain is a
dimension less quantity. However, for ease in understanding it is measured in micro
strain or (10 6 mm/mm). Damage Index (DI) is the area under the loading and divided by the chord modulus (Ec). DI and NLI are dimensionless quantities. All
unloading curves divided by the stress range. Non-linearity index (NLI) is the slope the parameters are calculated and averaged for the last four loading–unloading
of the chord of loading curve between half and one tenth of the maximum stress cycles.
 A. Nadeem et al. / Construction and Building Materials 38 (2013) 1058–1065 1061

3. Test results and discussions PC

50 80
FA40
In order to quantify the damage to concrete, the calculated SDT FA20
45
MK20
parameters (Ec, Eu, PS, NLI and DI) were averaged over the last four 70
MK10
of the five loading–unloading cycles. The calculations of the SDT for 40
Residual Ec (%)
this research are described as follows:

Residual Ec (%)
35 60

Ec (GPa)
 Ec is the chord slope of the loading curve between 30
0.637 N/mm2 and 6.366 N/mm2 stress level. 50
Ec (GPa)
 Eu is the chord slope of the unloading curve between the 25
maximum stress and a point 0.637 N/mm2 lower than the
20
maximum stress. 40
 PS is the plastic strain at 0.637 N/mm2 stress level. 15
 DI is the area of hysteresis between 0.637 N/mm2 and
30
6.366 N/mm2 stress level divided by the stress range. 10
 NLI is the chord slope of the loading curve between
0.637 N/mm2 and half the maximum stress divided by the 0 100 200 300 400 500
0
corresponding value of Ec. Temperature ( C)

Fig. 5. Variation in chord modulus with temperature for different concrete mixes.
Fig. 4 shows typical stress–strain relationship under low level of
cyclic loading of PC concrete heated to 200 °C, 300 °C and 400 °C
respectively. It is evident that load unload curves become gradually Before making comparison with relevant available literature, it
flat as the temperature increases. Therefore, the shape of the load– is noteworthy to mention here that according the literature [18]
unload curve can be used to give a rough idea of the degree of dam- initial modulus (Ei in Fig. 3) is more sensitive to degree of fracture
age to concrete specimens by fire [19]. Also, it can be deduced that than Ec. Therefore, severe loss in Ei is expected than Ec. Chang et al.
concrete is softening with elevated temperature [21]. In addition, determined the residual stress–strain relation for concrete after
the hysteresis loop became smaller with increasing number of cy- exposure to high temperature. The mixes were designed to have
cles suggesting less loss of energy during load–unload cycle [19]. compressive strength of 27 and 40 MPa respectively and were
heated at a rate of 1 to 4.5 °C/min with an increment of 0.5 °C/
min corresponding to temperature from 100 to 800 °C with an
3.1. Variation in chord modulus with temperature
increment of 100 °C. According to the equation proposed by the
authors, the loss in modulus of elasticity at 200 °C, 300 °C and
Chord loading modulus can be used to estimate permanent
400 °C was found to be 22%, 42% and 67% respectively. The loss
deflections of a structural member after fire. The percentage resid-
in chord modulus from exposure to high temperature is more for
ual stiffness of fire affected concrete would help in determining the
our case. This is due to the reason that compressive strength of
post firing load bearing capacity of structures [19]. Fig. 5 shows the
mixes made with PC, MK and FA (Table 2) is more than that pro-
variations of Ec with temperature for different concrete mixes. Ec
duced by Chang et al. It has been reported in literature [22] that
was found to decrease with increase in temperature. Metakaolin
at elevated temperature faster degradation occurs in properties
specimens had almost higher chord modulus than OPC and PFA
of HSC. Also, according to the literature [23], the temperature
mixes at all temperatures. The trend of loss is chord modulus
dependent destruction is more for the case of HSC than NSC be-
was almost similar in all concrete mixes. The Ec values of all mixes
cause cement paste in HSC must carry higher loads than NSC. In
appear to decrease from 37 to 47 GPa at 27 °C and from 12 to
addition, the variation in results may be due to different curing
15 GPa at 400 °C. All concrete mixes had almost similar chord
and heating regime as well as different heating rate.
modulus at 400 °C.
The relative loss in Ec with respect to the value at 27 °C for all
the mixes is nearly similar for each mix at a particular tempera- 3.2. Variation in unloading stiffness with temperature
ture. The loss in chord modulus at 200 °C, 300 °C and 400 °C is
up to 28%, 59% and 69% respectively. This shows that major loss Fig. 6 shows the variation of Eu with temperature for different
in Ec occur at 300 °C. concrete mixes. For all mixes, Eu decreases with increase in tem-
perature. At normal temperature, MK concrete mixes showed the
highest unloading stiffness. At 400 °C, there is little variation of
7
unloading stiffness among concrete mixes as compared with such
6 variation at other temperatures. The Eu of the mixes tested falls
from 65 GPa or over at 27 °C to 28–37 GPa at 400 °C.
5
Stress (MPa)

The information regarding the variation of the loss in Eu at ele-

4 vated temperatures with respect to unloading stiffness at normal
3 temperature for all the mixes is extracted from Fig. 6. The loss in
Eu values for mixes reach up to 15–30% at 200 °C, 38–62% at
2 300 °C and 51–63% at 400 °C. This shows that maximum loss in
1 Eu takes place up to 300 °C. There was no appreciable loss in Eu
for temperature above 300 °C. Also, MK mixes suffer the least rel-
0
0 100 200 300 400 500 600 700 800 ative loss at all temperatures.
It has been reported in the literature [24,25] that for similar
Mircostrain
conditions (mix design, curing and heating regime, heating rate
Fig. 4. Typical load–unload curves for PC concrete heated to 200 °C, 300 °C and and test conditions), mortar made with PC, MK and FA showed
400 °C. compressive strength loss of up to 10%, 16%, 39% and 75% at
1062 A. Nadeem et al. / Construction and Building Materials 38 (2013) 1058–1065

PC structures exposed to elevated temperatures can remain service-

100 FA40 80 able and repairable [27]. Also, among the concrete mixes, MK20
FA20 mix suffered the maximum increase in PS at elevated tempera-
90 MK20
70
tures. This is evident by presence of large pores in the SEM images
MK10
80 of MK20 at 400 °C (Figs. 8 and 9). In Fig. 8, the area between the
Residual Eu (%) large aggregate located on the right and the small aggregate A is

Residual Eu (%)
70 60 porous and for clarity is represented by R. In Fig. 9, the area be-
Eu (GPa)

tween large aggregate on the upper left side and a small aggregate
60 B located at a distance of 100 lm from large aggregate is porous
50
Ec (GPa) and is represented by S.
50
From Fig. 7, following additional information regarding the rel-
40 ative increase in PS of concrete mixes with respect to PS at normal
40
temperature is extracted. In relative terms, MK mixes showed the
30 least increase in PS as compared with other mixes although their
30 PS values were almost similar or slightly greater than the control
20 mix. FA and control mixes showed almost similar relative increase
0 100 200 300 400 500 in the PS up to 400 °C. The increase in PS varied from about 2 to 3
0
Temerature ( C) times at 200 °C, 5 to 8 times at 300 °C and 10 to 15 times at 400 °C.

Fig. 6. Variation in unloading stiffness with temperature for different concrete

mixes. 3.4. Variation in damage index with temperature

DI shows the energy loss in the load–unload loop. This is di-

200 °C, 400 °C, 600 °C and 800 °C respectively. It is clear that for
rectly related to the fractured state of the specimen and hence
same heat treatment, the reduction in elastic modulus is greater
gives a quantifiable way of measuring and comparing the damage
than compressive strength. This is consistent with the available lit-
by fire. It is evident from Fig. 10 that with increase of temperature,
erature [21,26].
damage index increases. Up to 200 °C, all concrete mixes have
relatively similar damage index and at higher temperatures the
3.3. Variation in plastic strain with temperature

Plastic strain may be used to estimate permanent deflections of

a structural member after fire. Fig. 7 shows that at 27 °C, the abso-
lute values of PS are small for all mixes. This is an indication of
dense microstructure of concrete specimens. At 200 °C, there is a
relatively small increase in PS for all concrete mixes thus the elas-
tic behavior of concrete is not much impaired at this temperature.
As the temperature increases, PS starts to increase rapidly which is
an indication that concrete is losing its integrity and deformations
are increasing enormously. It is also explained and supported by
the reduced chord modulus values at higher temperatures as dis-
cussed earlier. Major increase started at 300 °C and the increase
continued with the increase of temperature above 300 °C. At ele-
vated temperature, the PS in FA mixes was less than the MK mixes.
Thus, it may be feasible to increase the allowable working temper-
ature for FA mixes. This, in turn, means that a larger proportion of
Fig. 8. SEM image (600) of MK20 mix at 400 °C.

25 PC
FA40
FA20
20 MK20
MK10
Micro Plastic strain

15

10

0
0 100 200 300 400 500
0
Temerature ( C)

Fig. 7. Variation in PS with temperature for different concrete mixes. Fig. 9. SEM image (300) of MK20 mix at 400 °C.
 A. Nadeem et al. / Construction and Building Materials 38 (2013) 1058–1065 1063

PC Nassif et al. [19] through SDT assessed the damage to concrete

55 FA40 structures by fire. The mixes with water cement ratio of 0.45 were
FA20 given heat treatment at 217 °C, 240 °C, 287 °C, 320 °C, 378 °C and
50 MK20 470 °C. The loss in Ec at 320 °C and 378 °C was found to be 38%
MK10
and 73% while the loss in Eu at the above mentioned temperatures
45
was 26% and 60% respectively. DI with respect to normal tempera-
40 ture increased from 8 at 320 °C to 35 at 378 °C. In addition, PS ratio
Damage Index

at 320 °C and 378 °C was found to be 10 and 70 micro strain

35
respectively. In comparison to our results, the variation may be
30 due to different curing and heating regime as well as the difference
in mix design and materials used.
25
Also, according to the available literature [28], the disruption at
20 lower level of thermal exposure (less than 320 °C) is due to incom-
patibility between thermal deformations of the constituents caus-
15
ing microcracks to develop at the aggregate-cement paste interface
10 together with thermal profile arising from the temperature differ-
ence between the outer layer and the inner layers. For thermal
0 100 200 300 400 500 exposure higher than 320 °C, the decomposition of CSH into differ-
0
Temerature ( C) ent phases, dehydration of calcium hydroxide into free lime and
crystal transformation of quartz are the predominant damage
Fig. 10. Variation in DI with temperature for different mixes. mechanism [28,29].

3.6. Correlation between SDT parameters and elevated temperature

1.4
The correlation between SDT parameters and elevated temper-
PC
1.2 ature are shown in Figs. 5–7, 10 and 11. By looking at the width of
FA40
FA20 the band at each temperature, following can be deduced.
1.0 MK20
Non Linearity Index

MK10  PS and DI are more sensitive to concrete materials in the

0.8 higher temperature range than in the lower temperature
range.
0.6  Ec, Eu and NLI have almost similar sensitivity over the entire
range of temperature.
0.4
Apart from Ec, similar findings were found by Nassif [18] while
0.2 assessing and evaluating the performance of fire damaged con-
crete. According to the author, this lack of strong correlation be-
0.0 tween temperature and the SDT parameters signifies the
0 100 200 300 400 500 shortcomings of the existing techniques used in evaluating the
Temerature ( C)
0 post firing residual properties of concrete.

Fig. 11. Variation in NLI with temperature for different mixes. 3.7. Correlation between SDT parameters

In this section, the percentage residual stiffness of fire damaged

discrepancy between the DI of different mixes increases. In line
with other parameters, the major increase was at 300 °C and it
continued to increase with the increase of temperature. It is also
observed that at higher temperatures (300 °C and 400 °C), MK
mixes showed higher values of DI than FA mixes. Therefore, use
of MK mixes should be given careful thought in structures which
are subjected to simultaneous action of elevated temperature
and cycling loading. In addition, the relative increase in DI goes
as high as 4 times the unheated values with MK mixes showing
the highest relative increase values at 400 °C with respect to nor-
mal temperature.
3.5. Variation in non-linearity index with temperature
NLI determines the concavity of the loading–unloading hyster-
esis loop. NLI greater than one shows the concave up and less than
one shows concave down. Fig. 11 shows the variations of NLI with
temperature for different concrete mixes. NLI of control mix was
less than one at all temperatures which shows that its loading
unloading curve is going concave down. For all other mixes, the
NLI remained over one at other temperatures.
concrete is assessed through PS and DI measured by SDT. The cor-
relation between PS and DI with modulus of elasticity is graphi-
cally presented in Figs. 12 and 13. The coefficient of correlation
equal to 0.9657 suggest that PS and residual elastic modulus are
well correlated. The value of R2 for DI and residual elastic modulus
was found to be 0.9835, indicating strong correlation between
these parameters. Therefore, plastic strain and damage index mea-
sured from SDT can be used to estimate the percentage residual
chord loading modulus of concrete affected by fire [19]. It is worth
mentioning that the correlation of PS and residual elastic modulus
is very similar to that of DI and residual elastic modulus. This is due
to the reason that strong correlation appears between PS and DI as
shown in Fig. 14. The results are in agreement with Nassif findings
[18]. According to the author, DI and PS are well correlated with
residual elastic modulus. The coefficient of correlation was found
to be 0.91 and 0.96 for PS vs. residual elastic modulus and DI vs.
residual elastic modulus.
3.8. Classification system for fire damaged concrete
According to Nassif [18], fire damaged concrete based on the
strain energy dissipated in a hysteresis loop can be classified into
1064 A. Nadeem et al. / Construction and Building Materials 38 (2013) 1058–1065

Table 4
Categorization of HPC mixes based on classification system proposed by Nassif.

Mix SDT parameter Temperature (°C)

200 300 400
PC Ec II III V
PS II II IV
DI III V V
MK10 Ec II III V
PS II II IV
DI III V V
MK20 Ec II III V
PS II II IV
Fig. 12. Correlation of PS and residual chord modulus. DI IV V V
FA20 Ec II III V
PS I II III
DI III V V
FA40 Ec II III V
PS I II III
DI III V V

structures subjected to elevated temperatures. Based on the values

Fig. 13. Correlation of DI and residual chord modulus.
of DI, PC, MK10, FA20 and FA40 appear in Class III at 200 °C and
Class V at 300 °C and 400 °C respectively while MK20 appear in
class IV at 200 °C and in Class V at 300 °C and 400 °C respectively.
The HPC mixes that were made MK and FA showed variation in
the classification system proposed by Nassif [18]. The variation in
results may be due to the following reasons. (1) The classification
system by Nassif was based on mixes having 28 days compressive
strength of 52–70 MPa. However, in our case, the strength varied
from 85 to 112 MPa. (2) In our case, the mixes were made with
FA and MK while this was not the case for Nassif. (3) The classifi-
cation system proposed by Nassif was author’s judgment, which
can vary, based on the strain energy dissipated in a hysteresis loop
as well as the residual PS.

4. Conclusions

The results of SDT showed that it a good technique to quantita-

tively assess the damage occurring to the concrete because of the
Fig. 14. Correlation of PS and DI. effects of elevated temperatures. The SDT parameters are sensitive
measures of the change in the microstructure of concrete caused
by elevated temperatures in the temperature range tested. Based
on the results, following conclusions can be drawn.
Table 3
Classification system proposed by Nassif for fire damaged concrete [18].
 Collectively, the SDT parameters showed that the stiffness and
Damage Class of fire Plastic strain Most probable value of elasticity decreased and damage increased with the increase
Index damage (lstrain) residual stiffness
in temperature. The stiffness changes were evident from chord
Residual Ec Residual Ei modulus and unloading stiffness, elasticity changes from plastic
(%) (%) strain and damage to concrete from damage index.
<5 I <4.5 >76 >73  For all mixes, significant change in the SDT parameters occurred
5–10 II 4.5–11.4 76–51 73–40 at 300 °C. Therefore, 300 °C can be considered as critical
10–15 III 11.4–20 51–40 40–28
15–20 IV 20–30 40–34 28–22
temperature.
>20 V >30 <34 <22  At elevated temperatures (300 °C and 400 °C), FA mixes showed
lower values of plastic strain and damage index than MK mixes.
Thus, it can be used in places which are subjected to elevated
temperatures as observed in oil, gas, nuclear or power
five categories (Table 3). Based on this classification system, the industries.
mixes in this paper are categorized as shown in Table 4.  At elevated temperatures, MK mixes showed higher values of PS
According to Ec classification system, all the mixes appear in and DI. Therefore, use of MK mixes should be given careful
Class II, III and V at 200 °C, 300 °C and 400 °C respectively. Based thought in structures which are subjected to simultaneous
on PS classification system, PC, MK10 and MK20 appear in class action of elevated temperatures and cycling loading.
II at 200 °C and 300 °C while these mixes appear in Class IV at  The correlation of PS and DI with residual elastic modulus was
400 °C. FA20 and FA40 appear in Class I, II and III at 200 °C, remarkably well with values of coefficient of correlation equal
300 °C and 400 °C respectively. It appears that in comparison to to 0.9657 and 0.9835 respectively. Therefore, plastic strain
PC and MK mixes, FA mixes performed well and can be used in and damage index measured from SDT can be used to estimate
 A. Nadeem et al. / Construction and Building Materials 38 (2013) 1058–1065
the percentage residual chord loading modulus of concrete
affected by fire. This will help the practitioners who are con-
cerned with the reinstatement of fire damage structures. In
addition, knowing the residual properties will help in determin-
ing the load bearing capacity of structures.
5. Recommendations
HPC made with FA and MK showed variation in the classifica-
tion system proposed by Nassif. It is therefore suggested that fur-
ther work should be carried out in this area especially by taking
into account the secondary raw materials utilized in concrete so
as to have unified Classification system for HPC. Full range of re-
sults obtained from SDT thus would help in understanding the con-
dition of fire damaged concrete. In addition, validation should be
carried out on concrete members after exposure to real or simu-
lated fires.
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