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Since concrete is a consistently reliable building material, its importance to all nations' economies cannot be overstated.
However, the cement and concrete industries continue to generate massive amounts of waste which results in the emission of
carbon dioxide which is one of the environmental issues. Therefore, reducing the amount of cement is important by partially
replacing one of the waste materials. In this research; two municipal materials were used as alternatives for cement. It is
considered available in quantities with appropriate price as compared to other mineral materials. In addition, this research was
interest given to assess the strengths and durable behaviour of concrete production with these addition materials. The amount of
metakaolin used is (1-15) wt% and alum (1-5) wt% of cement. The central composite design (CCD) method was used in conjunction
with the response surface method to design concrete mixtures for this research and to analyse the results obtained from laboratory
tests. An empirical model was given for compressive strength, bulk density and splitting tensile strength. All concrete specimens
were cured after 7 and 28 days. The best results were found when metakaolin was used between (1-3) wt% and alum sludge
between (1.6-3) wt% as mixed materials to produce concrete and as a partial replacement of cement.
Keywords: Metakaolin; Alum sludge; Concrete; Minitab software; Compressive strength; Splitting tensile strength; Durability
1. Introduction energy use and CO2 emissions [8, 9 and 10]. From
the literature review, it has been found that
The industry of construction is growing fast metakaolin negatively influences the workability of
around the world. The huge growth in construction concrete which decreases with increasing the
is driving an increase in the demand for building replacement percentage of metakaolin until 15%
materials. Concrete is one of importance of the due to its high fineness. It has also been found that
building materials used in the industrial countries. the strength of metakaolin has been remarkably
Even though cement, aggregates, and water are all increased when replacing the cement with
integral constituents that must be used in the metakaolin from 10 to 15% compared to the poor
creation of concrete, the energy needed to produce effect of replacement ratios from 15 to 20% [11-15].
cement makes it expensive and harmful to the Therefore, the utilization of metakaolin as a
environment. Too much of a challenge has been supplementary cementitious material is considered
faced by the researchers to find varying alternatives beneficial in terms of environmental, technical and
or supplementary construction materials. These economic issues. Another alternative construction
may be characterized by cheaper, recycled and material in terms of reducing environmental impact
environmentally friendly materials to manufacture and saving costs is alum sludge. This material is a
concrete that is more durable, the life cycle of good final waste generated from the plant for drinking
strength that affects the cost of long-lasting it [1-4]. water treatment and is not considered a natural
Metakaolin is one of the alternative building pozzolanic material. Because of differences in
materials that is frequently used as a mineral source water and chemical composition from one
admixture to assist concrete to have better plant to the next, alum sludge is classified as a by-
properties, produce at a lower cost, and emit less product material [16-18].
CO2 due to the creation of the cement that is used Over the last decades, the waste water
in its production [5, 6 and 7]. It is a natural treatment plant has increased and had a negative
pozzolainc material [8]. The main advantages of this effect on the environment. Sludge is one of the main
material include its capacity to increase concrete wastes that are difficult to dispose of in an
strength and its high efficiency when used as a environmentally friendly manner and produces a lot
partial replacement for cement [5]. All experimental of pollution [19,20]. Much research has been done
testing indicated that mortar's sulphate resistance on the use of alum sludge in concrete to reduce the
had increased by around 30% and that concrete's harmful effects of this sludge on the environment. As
compressive strength had increased by about 50%. a result, it will lead to less cement being used while
Additionally, there has been a 40% reduction in still producing concrete with acceptable durability.
Autor corespondent/Corresponding author,
E-mail: hadel.obaidi@gmail.com
24 Hadel Obaidi, Ahlam Abdul-Rheem Farhan, Taha H. Abood Al-Saadi / Assessment of some mechanical properties for concrete
based on alum sludge and metakaolin
Previous research, for example, demonstrated that Alum sludge was obtained from Unity Water
the amount of sludge used in the concrete mixture Station in Iraq. It was dried under the sunshine
affects the strength and stiffness of the concrete [19- for 3 days, after that manually milled by using
21]. Another study has shown that the sludge was a steel hammer. Then, the powder dried in
subjected to heat treatment to reduce the harmful electric oven at 120°C for 3 hrs. Consequently,
materials and obtain the best concrete results [21]. removed any impurities particles from this
Sometime, it can use the sludge as partial powder by using sieving technique (No.200). It
replacement of sand or cement that depends on is noteworthy, the sieved alum sludge powder
particles size of them. The previous study showed was treated with 70% alcohol in order to
acceptable results for both replacements in different murder the harmful bacteria. Finally, the wet
percentages [20]. Many researchers have examined alum sludge powder dried at 120°C for 1 hr.
how to use the sludge in the production of building The resulted powder (off white color) has 2.34
and construction materials, for example, the as specific gravity. Table 4 represents the
production of brick, artificial aggregate, cement, and chemical compositions of resulted alum sludge
ceramics [22-26]. powder.
Some researchers have experimented with
Table 1
varying amounts of alum sludge as a partial Gradation of sand
replacement for cement to produce concrete with Iraqi specification
(2.5-15) % cement by weight. They found that the Opening size of sieve limits I.O.S.45/1984
Passing %
addition of it was between 6 to 7.5 % and improved (mm) Grading zone (2)
the strength of concrete after 7 and 28 curing days [28]
10 100 100
[4, 16 and 27]. From the literature, a lot of research 4.75 92.39 100-90
has shown reusing the sludge as a supplementary 2.36 75.21 100-75
material for cement in concrete but very limited 1.18 59.24 90-55
research has shown the use of metakaolin and alum 0.6 46.19 50-35
sludge together in it. 0.3 10.16 30-8
0.15 0.07 10-0
In this research, an attempt has been made
to produce a concrete mixture from alum sludge and
Table 2
metakaolin as cement partials in different Gradation of gravel
percentages and examine the main properties of Iraqi specification limits
concrete. This technique is beneficial to the Opening size of Passing
I.O.S.45/1984 (5/14 mm)
sieve (mm) %
environment by decreasing the waste that is [28]
disposed in landfills and it is also useful from the 20 100 100
14 94.5 100-90
economic perspective by producing concrete with
10 57.34 85-50
acceptable strength and durability. 5 0 10-0
Table 5
Codes used in the CCD for factors (independent variables) and their real experimental values
Table 7
The concrete mixes based on 1m3
Alum
Mix Cement Sand Gravel Metakaolin Water SP
Sludge W/C
No. Kg/m3 Kg/m3 Kg/m3 % L/m3 L/m3
%
R 485 820 748 0 0
1 484.95 820 748 3.050 1.586
2 484.85 820 748 12.95 1.586
3 484.92 820 748 3.050 4.414
4 484.82 820 748 12.95 4.414
5 484.96 820 748 1 3
6 484.82 820 748 15 3
182.4 4.365 0.37
7 484.91 820 748 8 1
8 484.87 820 748 8 5
9 484.98 820 748 8 3
10 484.98 820 748 8 3
11 484.98 820 748 8 3
12 484.98 820 748 8 3
13 484.98 820 748 8 3
3.3 Splitting tensile strength results At 28 days, the tensile strengths of mixes (2
As demonstrated in Fig. 3, the behavior of and 7) were approximately 3.21 and 3.98 MPa
concrete's tensile strength for all mixes was about respectively. When compared to the strength
the same as that of its compressive strength. results for mixes from (8 to13), the lowest values at
It is clear that the effects of the metakaolin 28 days dropped between 2.51 and 2.47 MPa.
and alum sludge additions on strength resulted in
mixes (1, 3, and 5) having acceptable strengths of 3.4 Analysis of variance (ANOVA)
around (4.54, 3.78, and 5.90) MPa at 28 days Table 8 illustrates the experimental results
respectively. While mixtures (4, 6) had significantly for all mixes studied by using variance analysis
decreased in tensile strength at 28 days, by around (ANOVA). Consequently, Tables (11, 12 and 13)
(0.47 and 0.40) MPa, respectively. present the findings. The experimental results are
used to build the regression model equations
28 Hadel Obaidi, Ahlam Abdul-Rheem Farhan, Taha H. Abood Al-Saadi / Assessment of some mechanical properties for concrete
based on alum sludge and metakaolin
Table 8
The matrix design along with the experimental results
Independent variables
Responses(dependent variables)
Coded Real
Exp. Y1
Meta Alum Y3
No. Y1 Predict Y2 Y2 Y3
X1 X2 Kaolin wt% Predict
Exp. ed Exp. Predicted Exp.
w% ed
1 -1 -1 3.050 1.586 44.77 42.206 2355 2355.306 4.54 4.851
2 1 -1 12.95 1.586 18.86 14.477 2344 2330.547 3.21 2.735
3 -1 1 3.050 4.414 27.82 29.651 2350 2363.953 3.78 4.455
4 1 1 12.95 4.414 2.13 2.138 2293 2293.194 0.47 0.360
5 -1.414 0 1 3 43.74 43.728 2377 2367.021 5.9 5.248
6 1.414 0 15 3 2.1 4.666 2290 2299.479 0.4 0.857
7 0 -1.414 8 1 24.46 28.841 2339 2348.399 3.98 4.128
8 0 1.414 8 5 13.07 11.237 2338 2328.101 2.52 2.169
9 0 0 8 3 15.27 16.399 2273 2281.600 1.77 1.606
10 0 0 8 3 17.67 16.399 2286 2281.600 1.47 1.606
11 0 0 8 3 15.73 16.399 2279 2281.600 1.65 1.606
12 0 0 8 3 16.22 16.399 2290 2281.600 1.55 1.606
13 0 0 8 3 17.1 16.399 2280 2281.600 1.59 1.606
Table 9
Analysis of variance for compressive strength Y1
Table 10
Analysis of variance for bulk density Y2
Table 11
Analysis of variance for splitting tensile strength Y3
Source DF Adj SS Adj MS F-Value P-Value
Metakaolin X1 1 19.2817 19.2817 83.50 0.000
Alum X2 1 3.8388 3.8388 16.62 0.005
X1X1 1 3.6367 3.6367 15.75 0.005
X2X2 1 4.1374 4.1374 17.92 0.004
X1X2 1 0.9794 0.9794 4.24 0.078
Pure Error 4 0.0501 0.0125
Total 12 32.5955
(second-order polynomial) that relate the response. The p-values for the coefficients in regression
As a result, three equations for compressive analysis reflect whether these relationships are
strength, bulk density and splitting tensile strength statistically significant. A low p-value (<0.05)
have been obtained. indicates that they are statistically different from
zero at the 95% confidence level. Therefore,
Where coefficients' p-values (<0.05) are statistically
Y1: Compressive Strength (MPa), Y2: bulk significant. Tables (11, 12 and 13) provide the F and
density (kg/m3), Y3: Splitting Tensile Strength P values for all linear, quadratic and interaction
(MPa) effects of the parameters. The smaller the value
Hadel Obaidi, Ahlam Abdul-Rheem Farhan, Taha H. Abood Al-Saadi / Assessment of some mechanical properties for concrete 29
based on alum sludge and metakaolin
Table 12
Summary of the response regression analysis
Response R2 (% ) Adjusted R2 (%) Predicted R2 SD
s (%)
Y1 96.92 94.72 79.16 2.979
Y2 94.02 89.76 63.71 11.494
Y3 95.04 91.50 65.59 0.481
of P, the bigger the magnitude of F and thus the The contour plot shows the best limits for the
more significant the corresponding coefficient term. replacement percentages of metakaolin and alum
The coefficients for the linear effect of the factors sludge, which ranged up to 2% of metakaoline and
metakaolin (p=0) and alum sludge (p=0.001) for the up to 1.8% of alum sludge, which contributed good
compressive strength are significant, as shown in strength to the concrete.
Table 9. The interaction between the variables From Fig 5 it can be observed more
metakaolin and alum sludge was not significant clarification of the results. The bulk density was
(p=0.972).Moreover, the quadratic effect of increased with decreasing the replacement
metakaolin (p=0.011) is significant, whereas it is percentage of metakaolin and alum sludge.
less so for alum sludge. The contour plot shows the area that gives a
For bulk density Table 10, the coefficients of low density when the percentages of addition of
all the effects of the factors were significant except metakaolin are between 8 to 13 and the alum
for the linear effect of alum (p=0.121) and the sludge percentages are between 2.7 to 4. This
interaction between the variables kaolin and alum agrees with mixes 4, 6, and 9.
(p=0.085). While the results for splitting tensile Figure 6 presents the effect of the
strength were all significant, except for the replacement percentage of metakaolin and alum
interaction between the variables kaolin and alum sludge on the splitting tensile strength. It can be
(p=0.078), as shown in Table 11. seen that strength values reduced with increasing
The regression equations in uncoded units are given in the proportions of metakaolin and alum sludge as
in Eqs. (2), (3) and (4). shown in 3D surface plot. In the contour plot, it can
be observed that the area represented by the
1- Compressive strength (Y1) = 70.48 - 5.360 X1 smallest triangle at the bottom and top on the left of
- 9.92 X2 + 0.1591 X12 + 0.910 X22 + 0.008 X1X2 the figure showed the best results of replacement
……… (2) percentages of about 2.5% of metakaolin with 1.6%
of alum sludge, and 2% of metakaolin with 4.4% of
2- Bulk density (Y2) = 2490.9 - 16.76 X1 - 76.9 X2 alum sludge respectively.
+ 1.054 X12 + 14.16 X22 - 1.643 X1X2 …… (3)
3.6 Durability results
3- Splitting tensile strength (Y3) = 9.25 - 0.574 X1
- 2.238 X2 + 0.02951 X12 + 0.3856 X22 In this research, this test was used to
- 0.0707 X1X2 ………. (4) determine the durability of concrete after 4 and 8
cycles of freezing and thawing. From Fig. 7, it can
The ANOVA for the three properties be seen that the pulse velocity of mixes (1, 3 and 5)
showed that the second-order polynomial model is higher than mixes (4 and 6) before and after
Eqs. (2), (3), and (4) is highly significant and subjecting to cycles of freezing and thawing. The
adequate to represent the actual relationship results showed decline in pulse velocity after
between the response and variables, with high subjecting the samples to cyclic freezing and
coefficients of determination (R2 = 96.92 %, 94.02 thawing. Where the decline of pulse velocity was
%, 95.04 %) for Y1, Y2, and Y3, respectively, as increased with increasing the number of cycles
shown in Table 12. These results indicate that the compared that of no cycles. The decrease of
three properties could be described well by the ultrasonic pulse velocity of mix (2 and 7) at 4 and 8
predicted model. cycle was approximately similar to that mixes from
8 to 13.
3.5 Plots of the 3D response surface and This may be happened due to the shrinkage
contours and expansion phenomena that was subjected to
The three regression equations (2), (3), and the samples during cycles of freezing and thawing.
(4) are presented by 3D response surface and This caused the generation of stresses resulting
contour plots, as shown in Figs.4, 5 and 6. from changing the volume of water in their pores
It can be seen from Fig. 4 that there is a inside the specimens, leading to a negative effect
sharp decline in the compressive strength values on the pulse velocity. This deterioration was clear
with increasing ratios for the metakaolin additive, that can be observed especially on mix (4 and 6).
while there is a slight increase in the compressive
strength value for alum sludge.
30 Hadel Obaidi, Ahlam Abdul-Rheem Farhan, Taha H. Abood Al-Saadi / Assessment of some mechanical properties for concrete
based on alum sludge and metakaolin
(a) (b)
Fig. 4- (a) 3D response surface and (b) contour plots of compressive strength (Y1) between alum sludge and metakaolin
(a) (b)
Fig.5- (a) 3D response surface and (b) contour plots of bulk density (Y2) between alum sludge and metakaolin
(a)
(b)
Fig. 6 - (a) 3D response surface and (b) contour plots of splitting tensile strength (Y3) between alum sludge and metakaolin
Hadel Obaidi, Ahlam Abdul-Rheem Farhan, Taha H. Abood Al-Saadi / Assessment of some mechanical properties for concrete 31
based on alum sludge and metakaolin
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