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Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33
www.ijera.com 28 | P a g e
A Study of the Pozzolanic Properties of Anfoega Kaolin
Tagbor, T, A., Boakye, K. A, Sarfo-Ansah J. and Atiemo, E.
CSIR-Building and Road Research Institute, Box UP 40, Kumasi, Ghana
Abstract
Kaolin, usually referred to as “hyire” in Ghana is commonly used for traditional religious ceremonies or
medicinal purposes. However, there exist abundant kaolin deposits in Ghana whose potential is under-utilized.
This work therefore has studied the potential use of kaolin from Anfoega, a small town in the Volta Region of
Ghana as a mineral admixture in Portland cement. The raw kaolin was calcined at 700o
C to produce metakaolin
and milled to cement fineness. The physical, chemical as well as mineralogical properties were conducted on the
raw and calcined kaolin. Compressive strength test on the mortars, prepared by replacing ordinary Portland
cement with 5% to 40% metakaolin was also conducted. XRF analysis of the metakaolin identified SiO2 and
Al2O3 as the dominant oxides whilst the presence of pyrophilites, magnetite and quartz were identified by XRD.
Compressive strength decreased as metakaolin content in the cement increased. The optimum replacement was
25%, recording compressive strengths of 11.2MPa, 16.8MPa and 43.0MPa for 2, 7 and 28 days respectively. At
25%, water permeability was improved by 38.7%. Co-efficient of water permeability (Kα) decreased with
increasing metakaolin content. This investigation has shown that Anfoega kaolin has good pozzolanic properties
and can be used as a mineral admixture in Portland cement.
Keywords: Kaolin, metakaolin, compressive strength, mineralogical composition, permeability
I. Introduction
Kaolin is a commercial term used to describe
white clay composed essentially of kaolinite,
Al4Si4O10(OH)8, with admixtures from quartz and
feldspar [1]. Although originally valued for use in the
manufacture of white ware ceramics, the principal
use of kaolin is now in the filling and coating of
paper. It is also used to a lesser extent as filler in
paint, rubber and plastics, as well as in a wide range
of other applications [2]. Kaolins are distinguished
from other clays by whiteness, and fine, controllable
particle size [1].
It is generally necessary to process kaolin from
the crude state in order to optimize these highly
commercial properties. When calcined between
temperatures of 500o
C and 850o
C, kaolin
dehydroxylates into metakaolin [3]. Metakaolin
reacts with Ca(OH)2, produces Calcium Silicate
Hydrates (CSH) gel at ambient temperature [4].
When mixed with Portland cement, the silica in the
metakaolin combines with the free lime released
during the hydration of cement [5]. The pozzolanic
activity is due to the presence of fairly divided glassy
silica and lime which produces calcium silicate
hydrate (C-S-H), C2ASH8 (gehlenite hydrate) and
C4AH13 (tetracalcium aluminate hydrate). The
formation of secondary C-S-H by this reaction
reduces total porosity and refines the pore structure,
improving the strength and impermeability of the
cementitious matrix [6, 7].
Pozzolanic materials including silica fumes, fly
ash, slag, rice husk ash and metakaolin have been
used in recent years as cement replacement for
developing high strength concrete with improved
workability, strength and durability [8, 9]. Anfoega in
the Volta Region of Ghana is well known for its vast
kaolin deposit covering about 160,000 square meters.
Kaolin, usually referred to as “hyire” or “white clay”
in Ghana is commonly used for traditional religious
ceremonies, medicinal purposes and sometimes eaten
by pregnant women to control the urge for vomiting.
II. Materials and methods
Materials
The materials used for this work were Kaolin
obtained from Anfoega, a small community about
250 km from Ho in the Volta Region of Ghana;
Ordinary Portland cement (Class 42.5N)
manufactured by Dangote Cement; Pit sand which
satisfied BS 4550: Part 6 [10] requirements. The sand
was sieved passing through 0.85 mm test sieve and
retained on 0.60 mm test sieve. The physical and
chemical properties of the kaolin, metakaolin, and
OPC are presented in Table 1 and 2 respectively.
Methods
The raw kaolin sample was prepared by taking
out various impurities and then air dried to get an
appreciable amount of moisture from the kaolin. It
was milled in a jaw crusher to an average particle
size of 150 µm. The milled kaolin sample was
nodulized and calcined in a laboratory kiln at 700 o
C
for 2 hours with a temperature rise increment rate of
5o
C/min to produce metakaolin. The calcined nodules
were milled to cement fineness using laboratory type
ball mill and sieved through 75µm standard sieve to
RESEARCH ARTICLE OPEN ACCESS
Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33
www.ijera.com 29 | P a g e
obtain powdered metakaolin (MK). The metakaolin
was used to replace 5%, 10%, 15%, 20%, 25%, 30%,
35% and 40% of ordinary Portland cement (OPC) to
produce blended cements. Physical properties such as
particle size distribution, Blaine fineness, specific
gravity and density were determined. Water demand,
setting times and soundness were determined
according to EN 196-3 [11]. The chemical and
mineralogical properties were also determined using
a Spectro Xlab X-Ray Fluorescence
spectrophotometer and PHILIPS PW 1830
diffractometer respectively. 70 mm × 70 mm mortar
cubes were molded according to procedures outlined
by EN 196-1 [12] and cured in a moisture cabinet.
The specimens were tested after 2, 7, 28 days. A
water permeability study was conducted using
methods prescribed by ASTM C642-06 [13].
III. Results and discussions
Physical properties
Figure 1 presents the particle size distribution
graph of the milled metakaolin whereas Table 1
shows some physical properties of the OPC,
metakaolin and the blended cements used in this
study. The particle size distribution, shown in Fig. 1
confirms that the sand used was very coarse and
contained minimal amount of silt. The metakaolin
was also very fine with 85% finer than 10 µm. The
Blaine indices in Table 1 shows that the surface area
of the blended cement increased as metakaolin
content in the mix increased. Specific gravity on the
other hand decreased with increasing metakaolin
content. Water demand to form a workable paste
increased with increase in the metakaolin content.
This is because the smaller particle size of the
metakaolin increased the surface area of the whole
mix translating into higher water demand [14]. There
was a progressive increase in both initial and final
setting times as the admixture content increased. At
40%, the initial and final setting times had increased
by 23.8% and 27% respectively. Setting time of
cements changes with particle size, specific surface
area and mineralogical structure of the cement
mixtures [15]. The increase could be due to the
decrease of tricalcium aluminate (C3A) content of the
OPC [16].
Figure 1: Particle size distribution of metakaolin and sieved sand
Table 1: Some physical properties of OPC, metakaolin and blended cements
Metakaolin replacement, %
Property OPC Metakaolin 5 10 15 20 25 30 35 40
specific gravity 3.18 2.69 3.20 3.05 3.00 2.96 2.94 2.9 2.87 2.82
Blaine fineness, m2
/kg 338 448 356 390 402 413 422 426 430 435
Water demand, % 28.3 – 29 32.5 33 33.4 35.2 39 36.2 36.5
Initial setting time, min 160 – 173 180 186 188 193 199 202 210
Final setting time, min 250 – 245 280 293 295 311 320 330 342
Soundness, mm 0.82 – 1.03 1.35 1.40 1.55 1.70 1.72 1.91 1.98
Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33
www.ijera.com 30 | P a g e
This results in slow hydration of the paste, thereby causing a delay in the setting of the paste. The
soundness of the blended cements also increased as metakaolin replacement increased. However, the setting
times and soundness obtained all fell within acceptable limits as prescribed by the EN 197-1 [17] standard.
Chemical and mineralogical analysis
The results of the chemical analysis of OPC, kaolin and metakaolin as determined by X-ray fluorescence
(XRF) have been presented in Table 2. For OPC, the sum of the CaO and SiO2 content gave 78.52% and loss on
ignition of 1.2% which satisfies the standard limit of EN 197–1[17].
Table 2: Chemical analysis of OPC, kaolin and metakaolin
Composition, % SiO2 Al2O3 Fe2O3 CaO MgO SO3 L.O.I
OPC 18.88 3.57 3.36 59.64 1.89 4.93 1.2
Kaolin 51.52 36.9 0.96 0.58 0.08 0.22 13
Metakaolin 57.5 40.18 1.23 0.45 0.12 0.61 0.65
Chemically, the OPC could be considered as good cement. Also, the SiO2 content of 51.52% and loss of
ignition of 0.65% of the metakaolin passed the requirements specified by the EN 197-1 [17]. The sum of SiO2,
Fe2O3 and Al2O3 content of the metakaolin exceeded the minimum value of 70% required by ASTM C618 [18].
Chemically, the metakaolin could also be considered as a good pozzolanic material. The XRD analysis in Fig. 2
shows that the kaolinite phase [Al2SiO5(OH)4.2H2O] was dominant with traces of quartz (SiO2). After
calcination (Fig. 3), more of the SiO2 phase was formed with Al2O3.4SiO2.H2O and Fe3O4 also present.
Figure 2: XRD of kaolin
Fig. 3: XRD of metakaolin
Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33
www.ijera.com 31 | P a g e
X-ray diffractograph obtained for the 28 days hydrated cement paste containing 25% metakaolin is shown
in Fig. 4. The main hydration products obtained are calcium disilicate [CaSi2O5], Portlandite [Ca(OH)2],
Tobermorite [Ca5Si6O16(OH)2] and sodium disilicate gel [Na2Si2O5].
Fig. 4: XRD of cement containing 25% metakaolin hydrated for 28 days
Compressive strength
The 2, 7 and 28 days compressive strength results of reference and blended cement shown in Fig. 5
indicates that all the OPC obtained a 2 and 7 days strengths of 22.5 MPa and 31.7 MPa respectively. These
strength values consistently reduced as the metakaolin replacement increased. The addition of 25% metakaolin
decreased strengths to 11.2 MPa and 16.8 MPa respectively, but still satisfied EN 197-1 [17] standard for early
strength. When the replacement was increased beyond 25%, the compressive strength consequently decreased,
satisfying the standard at 2 days but trailing it by 0.6MPa at 7 days. Beyond 30%, the mortar cubes recorded
compressive strengths lower than the EN 197-1 [17] standard for 7 days strength.
Figure 5: Compressive strength of OPC with different metakaolin contents
The reduction in strength is due to the slow reaction rate of the active metakaolin constituents with the
liberated Ca(OH)2 from the Portland cement [19]. When the curing period was increased to 28 days, the
reference cement sample recorded a compressive strength of 46.5 MPa. The strength values recorded for all
blended at 28 days were high, as even mortar cubes containing 40% metakaolin cement obtained compressive
strength that passed the ASTM C595 [20] standard. Thus 30% metakaolin cement satisfied requirements for
Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33
www.ijera.com 32 | P a g e
Class 42.5N cement whereas 40% metakaolin content performed as Class 32.5N cement. However, the optimum
replacement was 25% metakaolin, considering both early and ultimate strength.
Water permeability
The 28 days water permeability studies conducted on the reference and blended cements are presented in
Table 3. Co-efficient of water permeability, Kα, decreased as metakaolin content increased. The reference
cement obtained a co-efficient of water permeability of 5.32×10-10
m2
/s which was improved by about 38.7%
when the OPC was substituted with 25% metakaolin. At 40% metakaolin substitution, co-efficient of
permeability had decreased by 48.9%. Metakaolin acts as a filler and seals the pores in the mortar due to its high
degree of fineness [21]. It significantly influences the pore structure in mortars and produces substantial pore
refinement leading to significant modifications to the water transport properties [22].
Table 3: Water permeability studies on OPC and blended cements
Sample OPC 5% 10% 15% 20% 25% 30% 35% 40%
Kα×10-10
, m2
/s 5.32 5.12 4.83 4.52 4.01 3.26 3.13 3.01 2.72
Kα – Co-efficient of water permeability
IV. Conclusion
This study has shown that kaolin from Anfoega
has the relevant chemical content and when calcined
at 700o
C for 2 hours could be converted to
metakaolin. The metakaolin had a good chemical
composition satisfying the standard requirements of a
pozzolan. The mineralogical analysis of the
metakaolin showed the presence of more SiO2 phase
and traces of Al2O3.4SiO2.H2O and Fe3O4. The
hydrated cement containing metakaolin showed a
greater consumption of Ca(OH)2 than in the reference
cement with traces of unreacted Portlandite which
could be consumed if curing period is extended.
Compressive strength of blended cements increased
with increasing metakaolin content. 30% metakaolin
cement performed as Class 42.5N cement whereas
40% satisfied requirements of Class 32.5N cement.
The optimum replacement was 25% metakaolin,
considering both early and ultimate strength. Co-
efficient of water permeability also decreased with
increasing metakaolin content. This investigation has
shown that Anfoega kaolin has good pozzolanic
properties and can be used as a mineral admixture in
Portland cement.
References
[1] Bloodworth, A. J., Highley, D. E. and
Mitchell, C. J. (1993) Industrial Minerals
Laboratory Manual, Kaolin. A Report
prepared for the Overseas Development
Administration under the ODA/BGS
Technology Development and Research
Programme, Project 9 1/1, p.1.
[2] Talabi, A. O., Ademilua, O. L, and Akinola,
O. O. (2012) Compositional features and
industrial application of Ikere kaolinite,
Southwestern Nigeria, Research Journal in
Engineering and Applied Sciences, 1(5) 327-
333.
[3] Patil S. N., Gupta and A. K., Deshpande, S.
S., (2012): Metakaolin-Pozzolanic Material
for Cement in High Strength Concrete,
Journal of Mechanical and Civil Engineering
(IOSR-JMCE), 46-49.
[4] Poon, C. S., Lam, L., Kou, S. C., Wong, Y.
L., and Wong, R. (2001) Rate of pozzolanic
reaction in high-performance cement pastes,
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1306.
[5] Dojkov, I., Stoyanov, S., Ninov J. and
Petrov B. (2013) On the consumption of
lime by metakaolin, fly ash and kaolin in
model systems. Journal of Chemical
Technology and Metallurgy, 48 (1) 54-60.
[6] Siddique R. and Khan M. I. (2011),
Supplementary Cementing Materials.
Springer-Verlag Berlin Heidelberg, 179.
[7] Singh, M. and Garg, M. (2006), Reactive
pozzolana from India clays-their use in
cement mortars, Cement and concrete
research 36 (10) 1903-1907.
[8] Khater,H. M. (2010) Influence of
metakaolin on resistivity of cement mortar
to magnesium chloride solution. Ceramic –
Silicaty, 54 (4) 325-333.
[9] Kim H.S., Lee S.H. andMoon H.Y. (2007)
Strength properties and durability aspects of
high strength concrete using Korean
metakaolin. Construction and Building
Materials, 21 (6) 1229-1237.
[10] British Standards Institution (1978). Part 6:
Methods of testing cement: standard sand
for mortar cubes, p.23. BSI, London.
[11] European Standard EN 196-3 (2000),
Methods of testing cement: Determination
of setting times and soundness, p: 1-18.
European Committee for Standardization,
Brussels.
Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33
www.ijera.com 33 | P a g e
[12] European Standard EN 196-1 (2000),
Methods of testing cement: Determination
of strength, p: 1-36. European Committee
for Standardization, Brussels.
[13] American Standard for Testing and
Materials ASTM C642-06: Standard Test
Method for Density, Absorption, and Voids
in Hardened Concrete, ASTM, Philadelphia,
2006, p. 3.
[14] Memon, S. A., Arsalan, R., Khan, S., Lo, T.
Y. (2012) Utilization of Pakistani bentonite as
partial replacement of cement in concrete,
Construction and Building Materials, 30,
237-242
[15] Lea FM. The chemistry of cement and
concrete. 3rd ed. London: Edward Arnold,
Ltd.; Reprinted in 1976.
[16] Ambroise, J., Maximilien, S., Pera, J.
(1994), Properties of metakaolin blended
cements. Ad. Cem. Based Matter, 1(4) 161-
168.
[17] European Standard EN 197-1 (2000),
Composition, specifications and conformity
criteria for common cements, p: 15.
European Committee for Standardization,
Brussels.
[18] American Society for Testing and Materials
(2000), 2000 annual book of ASTM
standards: Part 14-C 618; Standard
specification for fly ash and raw or calcined
natural pozzolana for use as a mineral
admixture in Portland cement concrete,
p.355-358. ASTM, Philadelphia.
[19] Lea, F.M. (1970a), The chemistry of cement
and concrete, 3rd
ed., p: 235-245. Edward
Arnold (Publishers) Ltd., Glasgow.
[20] American Society for Testing and Materials
(2000) 2000 annual book of ASTM
standards: Part 14-C 595; Specification for
blended hydraulic cement, ASTM,
Philadelphia, 337-345.
[21] Guneyisi, E., Gesoglu, M., & Mermerdas, K.
(2008) Improving strength, drying
shrinkage, and pore structure of concrete
using metakaolin. Materials and Structures,
41, 937–949.
[22] Sabir, B. B., Wild, S., & Bai, J. (2001).
Metakaolin and calcined clays as pozzolans
for concrete: A review. Cement & Concrete
Composites, 23, 441–454.

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A Study of the Pozzolanic Properties of Anfoega Kaolin

  • 1. Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33 www.ijera.com 28 | P a g e A Study of the Pozzolanic Properties of Anfoega Kaolin Tagbor, T, A., Boakye, K. A, Sarfo-Ansah J. and Atiemo, E. CSIR-Building and Road Research Institute, Box UP 40, Kumasi, Ghana Abstract Kaolin, usually referred to as “hyire” in Ghana is commonly used for traditional religious ceremonies or medicinal purposes. However, there exist abundant kaolin deposits in Ghana whose potential is under-utilized. This work therefore has studied the potential use of kaolin from Anfoega, a small town in the Volta Region of Ghana as a mineral admixture in Portland cement. The raw kaolin was calcined at 700o C to produce metakaolin and milled to cement fineness. The physical, chemical as well as mineralogical properties were conducted on the raw and calcined kaolin. Compressive strength test on the mortars, prepared by replacing ordinary Portland cement with 5% to 40% metakaolin was also conducted. XRF analysis of the metakaolin identified SiO2 and Al2O3 as the dominant oxides whilst the presence of pyrophilites, magnetite and quartz were identified by XRD. Compressive strength decreased as metakaolin content in the cement increased. The optimum replacement was 25%, recording compressive strengths of 11.2MPa, 16.8MPa and 43.0MPa for 2, 7 and 28 days respectively. At 25%, water permeability was improved by 38.7%. Co-efficient of water permeability (Kα) decreased with increasing metakaolin content. This investigation has shown that Anfoega kaolin has good pozzolanic properties and can be used as a mineral admixture in Portland cement. Keywords: Kaolin, metakaolin, compressive strength, mineralogical composition, permeability I. Introduction Kaolin is a commercial term used to describe white clay composed essentially of kaolinite, Al4Si4O10(OH)8, with admixtures from quartz and feldspar [1]. Although originally valued for use in the manufacture of white ware ceramics, the principal use of kaolin is now in the filling and coating of paper. It is also used to a lesser extent as filler in paint, rubber and plastics, as well as in a wide range of other applications [2]. Kaolins are distinguished from other clays by whiteness, and fine, controllable particle size [1]. It is generally necessary to process kaolin from the crude state in order to optimize these highly commercial properties. When calcined between temperatures of 500o C and 850o C, kaolin dehydroxylates into metakaolin [3]. Metakaolin reacts with Ca(OH)2, produces Calcium Silicate Hydrates (CSH) gel at ambient temperature [4]. When mixed with Portland cement, the silica in the metakaolin combines with the free lime released during the hydration of cement [5]. The pozzolanic activity is due to the presence of fairly divided glassy silica and lime which produces calcium silicate hydrate (C-S-H), C2ASH8 (gehlenite hydrate) and C4AH13 (tetracalcium aluminate hydrate). The formation of secondary C-S-H by this reaction reduces total porosity and refines the pore structure, improving the strength and impermeability of the cementitious matrix [6, 7]. Pozzolanic materials including silica fumes, fly ash, slag, rice husk ash and metakaolin have been used in recent years as cement replacement for developing high strength concrete with improved workability, strength and durability [8, 9]. Anfoega in the Volta Region of Ghana is well known for its vast kaolin deposit covering about 160,000 square meters. Kaolin, usually referred to as “hyire” or “white clay” in Ghana is commonly used for traditional religious ceremonies, medicinal purposes and sometimes eaten by pregnant women to control the urge for vomiting. II. Materials and methods Materials The materials used for this work were Kaolin obtained from Anfoega, a small community about 250 km from Ho in the Volta Region of Ghana; Ordinary Portland cement (Class 42.5N) manufactured by Dangote Cement; Pit sand which satisfied BS 4550: Part 6 [10] requirements. The sand was sieved passing through 0.85 mm test sieve and retained on 0.60 mm test sieve. The physical and chemical properties of the kaolin, metakaolin, and OPC are presented in Table 1 and 2 respectively. Methods The raw kaolin sample was prepared by taking out various impurities and then air dried to get an appreciable amount of moisture from the kaolin. It was milled in a jaw crusher to an average particle size of 150 µm. The milled kaolin sample was nodulized and calcined in a laboratory kiln at 700 o C for 2 hours with a temperature rise increment rate of 5o C/min to produce metakaolin. The calcined nodules were milled to cement fineness using laboratory type ball mill and sieved through 75µm standard sieve to RESEARCH ARTICLE OPEN ACCESS
  • 2. Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33 www.ijera.com 29 | P a g e obtain powdered metakaolin (MK). The metakaolin was used to replace 5%, 10%, 15%, 20%, 25%, 30%, 35% and 40% of ordinary Portland cement (OPC) to produce blended cements. Physical properties such as particle size distribution, Blaine fineness, specific gravity and density were determined. Water demand, setting times and soundness were determined according to EN 196-3 [11]. The chemical and mineralogical properties were also determined using a Spectro Xlab X-Ray Fluorescence spectrophotometer and PHILIPS PW 1830 diffractometer respectively. 70 mm × 70 mm mortar cubes were molded according to procedures outlined by EN 196-1 [12] and cured in a moisture cabinet. The specimens were tested after 2, 7, 28 days. A water permeability study was conducted using methods prescribed by ASTM C642-06 [13]. III. Results and discussions Physical properties Figure 1 presents the particle size distribution graph of the milled metakaolin whereas Table 1 shows some physical properties of the OPC, metakaolin and the blended cements used in this study. The particle size distribution, shown in Fig. 1 confirms that the sand used was very coarse and contained minimal amount of silt. The metakaolin was also very fine with 85% finer than 10 µm. The Blaine indices in Table 1 shows that the surface area of the blended cement increased as metakaolin content in the mix increased. Specific gravity on the other hand decreased with increasing metakaolin content. Water demand to form a workable paste increased with increase in the metakaolin content. This is because the smaller particle size of the metakaolin increased the surface area of the whole mix translating into higher water demand [14]. There was a progressive increase in both initial and final setting times as the admixture content increased. At 40%, the initial and final setting times had increased by 23.8% and 27% respectively. Setting time of cements changes with particle size, specific surface area and mineralogical structure of the cement mixtures [15]. The increase could be due to the decrease of tricalcium aluminate (C3A) content of the OPC [16]. Figure 1: Particle size distribution of metakaolin and sieved sand Table 1: Some physical properties of OPC, metakaolin and blended cements Metakaolin replacement, % Property OPC Metakaolin 5 10 15 20 25 30 35 40 specific gravity 3.18 2.69 3.20 3.05 3.00 2.96 2.94 2.9 2.87 2.82 Blaine fineness, m2 /kg 338 448 356 390 402 413 422 426 430 435 Water demand, % 28.3 – 29 32.5 33 33.4 35.2 39 36.2 36.5 Initial setting time, min 160 – 173 180 186 188 193 199 202 210 Final setting time, min 250 – 245 280 293 295 311 320 330 342 Soundness, mm 0.82 – 1.03 1.35 1.40 1.55 1.70 1.72 1.91 1.98
  • 3. Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33 www.ijera.com 30 | P a g e This results in slow hydration of the paste, thereby causing a delay in the setting of the paste. The soundness of the blended cements also increased as metakaolin replacement increased. However, the setting times and soundness obtained all fell within acceptable limits as prescribed by the EN 197-1 [17] standard. Chemical and mineralogical analysis The results of the chemical analysis of OPC, kaolin and metakaolin as determined by X-ray fluorescence (XRF) have been presented in Table 2. For OPC, the sum of the CaO and SiO2 content gave 78.52% and loss on ignition of 1.2% which satisfies the standard limit of EN 197–1[17]. Table 2: Chemical analysis of OPC, kaolin and metakaolin Composition, % SiO2 Al2O3 Fe2O3 CaO MgO SO3 L.O.I OPC 18.88 3.57 3.36 59.64 1.89 4.93 1.2 Kaolin 51.52 36.9 0.96 0.58 0.08 0.22 13 Metakaolin 57.5 40.18 1.23 0.45 0.12 0.61 0.65 Chemically, the OPC could be considered as good cement. Also, the SiO2 content of 51.52% and loss of ignition of 0.65% of the metakaolin passed the requirements specified by the EN 197-1 [17]. The sum of SiO2, Fe2O3 and Al2O3 content of the metakaolin exceeded the minimum value of 70% required by ASTM C618 [18]. Chemically, the metakaolin could also be considered as a good pozzolanic material. The XRD analysis in Fig. 2 shows that the kaolinite phase [Al2SiO5(OH)4.2H2O] was dominant with traces of quartz (SiO2). After calcination (Fig. 3), more of the SiO2 phase was formed with Al2O3.4SiO2.H2O and Fe3O4 also present. Figure 2: XRD of kaolin Fig. 3: XRD of metakaolin
  • 4. Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33 www.ijera.com 31 | P a g e X-ray diffractograph obtained for the 28 days hydrated cement paste containing 25% metakaolin is shown in Fig. 4. The main hydration products obtained are calcium disilicate [CaSi2O5], Portlandite [Ca(OH)2], Tobermorite [Ca5Si6O16(OH)2] and sodium disilicate gel [Na2Si2O5]. Fig. 4: XRD of cement containing 25% metakaolin hydrated for 28 days Compressive strength The 2, 7 and 28 days compressive strength results of reference and blended cement shown in Fig. 5 indicates that all the OPC obtained a 2 and 7 days strengths of 22.5 MPa and 31.7 MPa respectively. These strength values consistently reduced as the metakaolin replacement increased. The addition of 25% metakaolin decreased strengths to 11.2 MPa and 16.8 MPa respectively, but still satisfied EN 197-1 [17] standard for early strength. When the replacement was increased beyond 25%, the compressive strength consequently decreased, satisfying the standard at 2 days but trailing it by 0.6MPa at 7 days. Beyond 30%, the mortar cubes recorded compressive strengths lower than the EN 197-1 [17] standard for 7 days strength. Figure 5: Compressive strength of OPC with different metakaolin contents The reduction in strength is due to the slow reaction rate of the active metakaolin constituents with the liberated Ca(OH)2 from the Portland cement [19]. When the curing period was increased to 28 days, the reference cement sample recorded a compressive strength of 46.5 MPa. The strength values recorded for all blended at 28 days were high, as even mortar cubes containing 40% metakaolin cement obtained compressive strength that passed the ASTM C595 [20] standard. Thus 30% metakaolin cement satisfied requirements for
  • 5. Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33 www.ijera.com 32 | P a g e Class 42.5N cement whereas 40% metakaolin content performed as Class 32.5N cement. However, the optimum replacement was 25% metakaolin, considering both early and ultimate strength. Water permeability The 28 days water permeability studies conducted on the reference and blended cements are presented in Table 3. Co-efficient of water permeability, Kα, decreased as metakaolin content increased. The reference cement obtained a co-efficient of water permeability of 5.32×10-10 m2 /s which was improved by about 38.7% when the OPC was substituted with 25% metakaolin. At 40% metakaolin substitution, co-efficient of permeability had decreased by 48.9%. Metakaolin acts as a filler and seals the pores in the mortar due to its high degree of fineness [21]. It significantly influences the pore structure in mortars and produces substantial pore refinement leading to significant modifications to the water transport properties [22]. Table 3: Water permeability studies on OPC and blended cements Sample OPC 5% 10% 15% 20% 25% 30% 35% 40% Kα×10-10 , m2 /s 5.32 5.12 4.83 4.52 4.01 3.26 3.13 3.01 2.72 Kα – Co-efficient of water permeability IV. Conclusion This study has shown that kaolin from Anfoega has the relevant chemical content and when calcined at 700o C for 2 hours could be converted to metakaolin. The metakaolin had a good chemical composition satisfying the standard requirements of a pozzolan. The mineralogical analysis of the metakaolin showed the presence of more SiO2 phase and traces of Al2O3.4SiO2.H2O and Fe3O4. The hydrated cement containing metakaolin showed a greater consumption of Ca(OH)2 than in the reference cement with traces of unreacted Portlandite which could be consumed if curing period is extended. Compressive strength of blended cements increased with increasing metakaolin content. 30% metakaolin cement performed as Class 42.5N cement whereas 40% satisfied requirements of Class 32.5N cement. The optimum replacement was 25% metakaolin, considering both early and ultimate strength. Co- efficient of water permeability also decreased with increasing metakaolin content. This investigation has shown that Anfoega kaolin has good pozzolanic properties and can be used as a mineral admixture in Portland cement. References [1] Bloodworth, A. J., Highley, D. E. and Mitchell, C. J. (1993) Industrial Minerals Laboratory Manual, Kaolin. A Report prepared for the Overseas Development Administration under the ODA/BGS Technology Development and Research Programme, Project 9 1/1, p.1. [2] Talabi, A. O., Ademilua, O. L, and Akinola, O. O. (2012) Compositional features and industrial application of Ikere kaolinite, Southwestern Nigeria, Research Journal in Engineering and Applied Sciences, 1(5) 327- 333. [3] Patil S. N., Gupta and A. K., Deshpande, S. S., (2012): Metakaolin-Pozzolanic Material for Cement in High Strength Concrete, Journal of Mechanical and Civil Engineering (IOSR-JMCE), 46-49. [4] Poon, C. S., Lam, L., Kou, S. C., Wong, Y. L., and Wong, R. (2001) Rate of pozzolanic reaction in high-performance cement pastes, Cement and Concrete Research, 31:1301- 1306. [5] Dojkov, I., Stoyanov, S., Ninov J. and Petrov B. (2013) On the consumption of lime by metakaolin, fly ash and kaolin in model systems. Journal of Chemical Technology and Metallurgy, 48 (1) 54-60. [6] Siddique R. and Khan M. I. (2011), Supplementary Cementing Materials. Springer-Verlag Berlin Heidelberg, 179. [7] Singh, M. and Garg, M. (2006), Reactive pozzolana from India clays-their use in cement mortars, Cement and concrete research 36 (10) 1903-1907. [8] Khater,H. M. (2010) Influence of metakaolin on resistivity of cement mortar to magnesium chloride solution. Ceramic – Silicaty, 54 (4) 325-333. [9] Kim H.S., Lee S.H. andMoon H.Y. (2007) Strength properties and durability aspects of high strength concrete using Korean metakaolin. Construction and Building Materials, 21 (6) 1229-1237. [10] British Standards Institution (1978). Part 6: Methods of testing cement: standard sand for mortar cubes, p.23. BSI, London. [11] European Standard EN 196-3 (2000), Methods of testing cement: Determination of setting times and soundness, p: 1-18. European Committee for Standardization, Brussels.
  • 6. Tagbor, T. A. et al. Int. Journal of Engineering Research and Applications www.ijera.com ISSN: 2248-9622, Vol. 5, Issue 8, (Part - 1) August 2015, pp.28-33 www.ijera.com 33 | P a g e [12] European Standard EN 196-1 (2000), Methods of testing cement: Determination of strength, p: 1-36. European Committee for Standardization, Brussels. [13] American Standard for Testing and Materials ASTM C642-06: Standard Test Method for Density, Absorption, and Voids in Hardened Concrete, ASTM, Philadelphia, 2006, p. 3. [14] Memon, S. A., Arsalan, R., Khan, S., Lo, T. Y. (2012) Utilization of Pakistani bentonite as partial replacement of cement in concrete, Construction and Building Materials, 30, 237-242 [15] Lea FM. The chemistry of cement and concrete. 3rd ed. London: Edward Arnold, Ltd.; Reprinted in 1976. [16] Ambroise, J., Maximilien, S., Pera, J. (1994), Properties of metakaolin blended cements. Ad. Cem. Based Matter, 1(4) 161- 168. [17] European Standard EN 197-1 (2000), Composition, specifications and conformity criteria for common cements, p: 15. European Committee for Standardization, Brussels. [18] American Society for Testing and Materials (2000), 2000 annual book of ASTM standards: Part 14-C 618; Standard specification for fly ash and raw or calcined natural pozzolana for use as a mineral admixture in Portland cement concrete, p.355-358. ASTM, Philadelphia. [19] Lea, F.M. (1970a), The chemistry of cement and concrete, 3rd ed., p: 235-245. Edward Arnold (Publishers) Ltd., Glasgow. [20] American Society for Testing and Materials (2000) 2000 annual book of ASTM standards: Part 14-C 595; Specification for blended hydraulic cement, ASTM, Philadelphia, 337-345. [21] Guneyisi, E., Gesoglu, M., & Mermerdas, K. (2008) Improving strength, drying shrinkage, and pore structure of concrete using metakaolin. Materials and Structures, 41, 937–949. [22] Sabir, B. B., Wild, S., & Bai, J. (2001). Metakaolin and calcined clays as pozzolans for concrete: A review. Cement & Concrete Composites, 23, 441–454.