Darryn Kisten Dissertation

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ALTERNATIVE MATERIALS FOR CONCRETE

An investigation into the influence of metakaolin in


conventional concrete.

BY

DARRYN KISTEN

213506133

Submitted in partial fulfillment of the academic requirement for the degree of Bachelor
Science in Civil Engineering, University of KwaZulu-Natal

School of Civil Engineering, Surveying and Construction

University of KwaZulu-Natal

Durban, November 2018


ABSTRACT

The construction industry has been put on the spotlight for its influence on the social,
economic and environmental factors globally. The cement and concrete industry in
particular has an enormous impact on the environment due to its copious CO2 emissions.

The need for alternative materials for concrete is generating a great deal of attention and
resulting in extensive research being initiated. Research into industrial wastes as
supplementary cementitious materials has been proved to be effective in reducing the
effect of cement on the environment. However, these secondary products are not readily
available in surplus and results in the need to find alternative sources of supplementary
cementitious materials.

The use of pozzolans have been used in ancient time by the Romans and are seen to be
quite effective due to the fact that they are still existing today. Focus on the use of
pozzolans has introduced the use of metakaolin, a calcined clay as an innovative
supplementary material. The use of metakaolin has been noted to increase the overall
strengths of concrete and enhance the durability significantly.

This research investigates the influence of metakaolin in concrete at various percentage


additions (0%; 5%, 10%, 15% and 20% metakaolin replacement of cement). The
experimental methods assess the fresh properties, mechanical properties and durability
properties of the concrete to determine if it is a suitable cement replacement material. The
study concludes that use of metakaolin does in fact improve mechanical and durability
properties of the concrete substantially and can be vital component in the future of
sustainable concrete by combining it with other supplementary cementitious materials.

Keywords: Metakaolin, Supplementary cementitious materials, concrete, sustainability,


calcined clay, pozzolan.

i
DECLARATION
I, Darryn Kisten declare that

(i) The research reported in this dissertation, except where otherwise indicated is my
original work.

(ii) This dissertation has not been submitted for a degree or examination to any other
university.

(iii) This dissertation does not contain other person’s data, pictures, graphs or other
information, unless specifically acknowledged as being sourced from other
persons.

(iv) This dissertation does not contain other person’s writing, unless specifically
acknowledged as being sourced from other researchers. Where other written
sources have been quoted, then:

(a) their words have been re-written but in general information attributed to
them has been referenced;

(b) where the exact words have been used, their writing has been placed inside
quotation marks, and referenced.

(v) Where I have reproduced a publication of which I am an author, co-author or


editor, I have indicated in detail which part of the publication was actually written
by myself alone and have fully referenced such publications.

(vi) This dissertation does not contain text, graphics or tables copied and pasted from
the Internet, unless specifically acknowledged and the source being detailed in the
dissertation and in the Reference sections.

Name : Darryn Kisten

Student number : 213506133

Signature : ………………………………….

Date : ………………………………….

ii
DEDICATION

“This dissertation is dedicated to my mum, Diana Kisten who has


persevered and strived to the best of her ability to ensure that her children
have everything they dreamed of in life. May God continue to shower his
richest blessings upon you. You are truly a Proverbs 31 woman.

Thank you mum!”

iii
ACKNOWLEDGEMENTS
First and foremost; all thanks, honor and glory is to God who has been the source of my
success and reason I am able to present this dissertation. (Jeremiah 29:11)

I would like to thank my supervisor, Dr. M.W. Kiliswa for his support, guidance and
introduction to metakaolin. I would like to acknowledge the laboratory staff and
technicians (Mr. Ishaan Ramlakan and Ms. Tejasvini Ramkisoon) for their help and
assistance and the University of Kwa-Zulu Natal including all other staff that assisted in
accomplishing this task.

Special thanks goes to Prof. P. Everitt for introducing me to concrete fundamentals and
developing my interest in this field. Additional thanks must be given to the staff of
Naidu Consulting for providing their expertise and testing equipment for the
permeability tests; and the staff at UKZN Westville campus for their assistance and use
of the microscopy analysis.

I would like to express my sincerest gratitude to Savio Hageman and the Kaolin Group
for sponsoring the 25 kg of KG-K40 High-Reactivity Metakaolin which was an
essential part of the research. I would also like to acknowledge Serina Trading
Company for their referral to the Kaolin Group.

My sincerest thanks and heartfelt gratitude goes out to the following people for their
assistance, valuable time, support, advice and motivation.

My parents (Diana and Ashley Kisten), sister (Rene’ Kisten), aunt and uncle (Audrey
and Rishi Sewram) and grandparents (Sunny and Gladys Chetty) for their continual
support, advice and guidance in developing me into the person I am today.
(Proverbs 22:6).

Tamlyn Jade Chetty for her endearing love; advice, motivation and encouragement and
her inexhaustible support and assistance during this period.

Pastor Noel Theophilus for his Godly guidance, advice and prayer.

Deveshan Pillay, Sean Moodley, Abish Gopal, Yashin Sookai, Olivia Sookdeo
Merushka Chetty, Mikaar Singh, and other colleagues from university, for their
assistance, advice and influence in my life.

iv
TABLE OF CONTENTS
ABSTRACT....................................................................................................................... i

DECLARATION .............................................................................................................. ii

DEDICATION ................................................................................................................. iii

ACKNOWLEDGEMENTS ............................................................................................. iv

LIST OF FIGURES ......................................................................................................... ix

LIST OF TABLES .......................................................................................................... xii

CHAPTER 1: INTRODUCTION ..................................................................................... 1

1.1. Research background and significance .............................................................. 1

1.1.1. Research background ...................................................................................... 1

1.1.2. Research significance ..................................................................................... 2

1.2. Research question................................................................................................... 3

1.3. Research aims......................................................................................................... 3

1.4. Research objectives ................................................................................................ 3

1.5. Research methodology ........................................................................................... 4

1.6. Dissertation outline ................................................................................................ 4

CHAPTER 2: LITERATURE REVIEW .......................................................................... 6

2.1. Introduction ............................................................................................................ 6

2.2. Conventional concrete ............................................................................................ 7

2.2.1. Environmental concerns ................................................................................. 7

2.2.2. Chemical and Mechanical properties .............................................................. 8

2.3. Supplementary cementitious materials and partial cement replacements .............. 9

2.4. Metakaolin............................................................................................................ 11

2.4.1. Background and properties ........................................................................... 11

2.4.2. Physical properties of metakaolin ................................................................. 12

2.4.3. Chemical composition of metakaolin ........................................................... 12

2.4.4. Processing of metakaolin and high reactivity metakaolin. ........................... 12

v
2.4.5. Influence of metakaolin on conventional concrete ....................................... 14

2.4.6. Past research ................................................................................................. 20

2.4.7. Metakaolin in South Africa........................................................................... 24

2.5. Chapter summary ................................................................................................. 25

2.5.1. Mechanical properties ................................................................................... 25

2.5.2. Durability ...................................................................................................... 25

2.5.3. Rheology and workability............................................................................. 25

2.5.4. Water requirement. ....................................................................................... 25

2.5.5. Finishing ....................................................................................................... 26

2.5.6. Experimental methods .................................................................................. 26

CHAPTER 3: METHODOLOGY .................................................................................. 27

3.1. Introduction .......................................................................................................... 27

3.2. Materials and their properties............................................................................... 27

3.2.1. Cement .......................................................................................................... 27

3.2.2. Fine aggregate ............................................................................................... 27

3.2.3. Coarse aggregate ........................................................................................... 28

3.2.4. Metakaolin .................................................................................................... 29

3.2.5. Water ............................................................................................................. 30

3.2.6. Moulds for concrete samples ........................................................................ 30

3.3. Conceptual mix design ......................................................................................... 31

3.4. Mixing and preparation of samples ...................................................................... 32

3.4.1. Mixing the concrete ...................................................................................... 32

3.4.2. Workability – Slump test .............................................................................. 33

3.5. Experimental testing............................................................................................. 34

3.5.1. Mechanical properties - Compression test .................................................... 34

3.5.2. Mechanical properties - Flexural tests .......................................................... 35

3.5.3. Durability – Density, Water Absorption and sorptivity................................ 36

vi
3.5.4. Durability – Air/Water permeability............................................................. 38

3.5.5. Scanning Electron Microscope (SEM) ......................................................... 40

3.6. Chapter summary ................................................................................................. 40

CHAPTER 4: RESULTS AND DISCUSSION.............................................................. 41

4.1. Introduction .......................................................................................................... 41

4.2. Material properties ............................................................................................... 41

4.2.1. Fineness modulus by sieve analysis.............................................................. 41

4.2.2. Coarse aggregate ........................................................................................... 42

4.2.3. Water-Binder ratio and water requirement ................................................... 42

4.3. Mix design ............................................................................................................ 42

4.4. Fresh mix properties ............................................................................................. 43

4.5. Mechanical properties .......................................................................................... 46

4.5.1. Compression strength ................................................................................... 46

4.5.2. Flexural strength ........................................................................................... 49

4.5.3. Further Evaluation ........................................................................................ 51

4.6. Durability ............................................................................................................. 52

4.6.1. Mass, Density and absorption ....................................................................... 52

4.6.2. Water sorptivity ............................................................................................ 53

4.6.3. Air Permeability ............................................................................................ 54

4.6.4. Water permeability ....................................................................................... 55

4.7. Scanning Electron Microscope ............................................................................ 55

4.8. Limitations and Errors.......................................................................................... 58

4.9. Chapter Summary................................................................................................. 59

CHAPTER 5: CONCLUSION AND RECOMMENDATIONS .................................... 60

5.1. Conclusion............................................................................................................ 60

5.1.1. Fresh mix properties ..................................................................................... 60

5.1.2. Mechanical properties ................................................................................... 61

vii
5.1.3. Durability ...................................................................................................... 61

5.1.4. Environmental, economic and social impacts............................................... 63

5.2. Recommendations ................................................................................................ 64

5.3. Future scope/research ........................................................................................... 64

REFERENCES ............................................................................................................... 65

APPENDICIES ............................................................................................................... 70

APPENDIX A: Data and pre mix calculations ........................................................... 70

A.1. Water-Binder ratio vs Strength ....................................................................... 70

A.2. Sample Calculations........................................................................................ 71

A.3. Metakaolin Pricing .......................................................................................... 77

APPENDIX B: Tabulated results and raw data .......................................................... 78

B.1. Fineness modulus by sieve analysis ................................................................ 78

B.2. Fresh concrete properties ................................................................................ 78

B.3. Mechanical properties ..................................................................................... 78

APPENDIX C: Pictures from research ....................................................................... 89

APPENDIX D: ECSA Outcomes................................................................................ 94

viii
LIST OF FIGURES
Figure 1: Durability vs Time and expenditure (The Concrete Institute, 2013) ................ 2
Figure 2: The Pantheon (Rolling Rome S.R.L, 2014) ...................................................... 6
Figure 3: Deteriorated column (National Research Council of Canada, 2003) ................ 7
Figure 4: Deteriorated bridge (Shimomura, 2004) ........................................................... 7
Figure 5: CO2 emissions from cement production (Hokfors, 2014) ................................ 8
Figure 6: Contribution of deterioration mechanisms (Basheer et al., 1996) ..................... 9
Figure 7: Supplementary cementitious materials(Portland Cement Association, 2018) 10
Figure 8: Kaolinite (Rashad, 2013)................................................................................. 11
Figure 9: Kaolinite Structure (Rashad, 2013) ................................................................. 11
Figure 10: Production of metakaolin by flash calcination (Cassagnabere et al., 2010).. 13
Figure 11: The filler effect (Wiggins, 2011)................................................................... 14
Figure 12: Calcium hydroxide content for metakaolin replacement (Sabir et al., 2001) 15
Figure 13: Metakaolin compressive strength (Whitemud World Cement, 2010)........... 16
Figure 14: Metakaolin ASR mitigation (Whitemud World Cement, 2010) ................... 16
Figure 15: Slump comparison (Wiggins, 2011).............................................................. 17
Figure 16: Metakaolin CO2 footprint (Whitemud World Cement, May 2010) .............. 18
Figure 17: Concrete production costs (Vancouver, 2002) .............................................. 19
Figure 18: Kaolin deposits in Africa (Ekosse, 2010)...................................................... 24
Figure 19: Kaolin deposits in Southern Africa (Ekosse, 2010) ...................................... 24
Figure 20: Specified sieves ............................................................................................. 28
Figure 21: Vibrating machine ......................................................................................... 28
Figure 22: Metakaolin KG-K40 analysis (Kaolin-Group, 2018) .................................... 29
Figure 23: High reactivity KG K40 Metakaolin ............................................................. 29
Figure 24: Slump test (Big Pics, 2018) ........................................................................... 33
Figure 25: Cube in compression test............................................................................... 34
Figure 26: Flexural strength test (SANS, 2006) ............................................................. 35
Figure 27: Beam in the flexural strength test .................................................................. 36
Figure 28: Cored sample ................................................................................................. 37
Figure 29: Water sorptivity setup ................................................................................... 37
Figure 30: Air permeability ............................................................................................ 39
Figure 31: Water permeability ........................................................................................ 39
Figure 32: LEO 1450 SEM ............................................................................................. 40

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Figure 33: Rotary pumped coater ................................................................................... 40
Figure 34: Fine aggregate grading curve ........................................................................ 41
Figure 35: Slump for 0% MK ......................................................................................... 43
Figure 36: Slump for 15%MK ........................................................................................ 43
Figure 37: Water binder ratio used ................................................................................ 43
Figure 38: Fresh mix properties ...................................................................................... 44
Figure 39: Fresh mix temperature ................................................................................... 45
Figure 40: Compressive strength over time .................................................................... 46
Figure 41: Compressive strengths vs percentage metakaolin ......................................... 47
Figure 42: 28th day compressive strength comparison.................................................... 48
Figure 43: Flexural strength over time ........................................................................... 49
Figure 44: Flexural strengths vs percentage metakaolin ................................................ 50
Figure 45: 28 day percentage increase in strengths ........................................................ 51
Figure 46: Average dry density ...................................................................................... 52
Figure 47: Mass and water absorption ............................................................................ 53
Figure 48: Water sorptivity ............................................................................................. 54
Figure 49: 0% Metakaolin content.................................................................................. 55
Figure 50: 5% Metakaolin content.................................................................................. 56
Figure 51: 10% Metakaolin content................................................................................ 56
Figure 52: 15% Metakaolin content................................................................................ 57
Figure 53: 20% Metakaolin content................................................................................ 57
Figure 54 : Water-Cement ratios for desired strengths ................................................... 70
Figure 55: 0% metakaolin mix design ............................................................................ 72
Figure 56: 5% metakaolin mix design ............................................................................ 73
Figure 57: 10% metakaolin mix design .......................................................................... 74
Figure 58: 15% metakaolin mix design .......................................................................... 75
Figure 59: 20% metakaolin mix design .......................................................................... 76
Figure 60: Metakaolin pricing from Serina Trading Company ...................................... 77
Figure 61: Actual vs NPC estimated strengths ............................................................... 80
Figure 62: Average density ............................................................................................. 81
Figure 63: Average mass ................................................................................................ 81
Figure 64: Water absorption rate .................................................................................... 82
Figure 65: Water sorptivity summary- O%MK .............................................................. 84
Figure 66: 0% MK - Mwt vs √hr .................................................................................... 84

x
Figure 67: Water sorptivity summary- 5%MK ............................................................... 85
Figure 68: 5% MK - Mwt vs √hr .................................................................................... 85
Figure 69: Water sorptivity summary- 10%MK ............................................................. 86
Figure 70: 10% MK - Mwt vs √hr .................................................................................. 86
Figure 71: Water sorptivity summary- 15%MK ............................................................. 87
Figure 72: 15% MK - Mwt vs √hr .................................................................................. 87
Figure 73: Water sorptivity summary- 20%MK ............................................................. 88
Figure 74: 20% MK - Mwt vs √hr .................................................................................. 88
Figure 75: KG K40 high reactivity metakaolin .............................................................. 89
Figure 76: Fine and coarse aggregate for the mix .......................................................... 89
Figure 77: Weighing material ......................................................................................... 89
Figure 78: Tilting mixing drum ...................................................................................... 89
Figure 79: Slump test ...................................................................................................... 89
Figure 80: Moulds on vibrating table ............................................................................. 89
Figure 81: Fresh concrete in cube mould........................................................................ 90
Figure 82: Fresh concrete in beam mould ...................................................................... 90
Figure 83: Wet controlled curing .................................................................................... 90
Figure 84: Wet and damp curing .................................................................................... 90
Figure 85: Compression test ........................................................................................... 90
Figure 86: Abnormal failure of cube .............................................................................. 90
Figure 87: Coring from cubes ......................................................................................... 91
Figure 88: Drying discs in oven ...................................................................................... 91
Figure 89: Mixing Calcium hydroxide solution ............................................................. 91
Figure 90: Slices for SEM imaging ................................................................................ 91
Figure 91: 0% Metakaolin cube ...................................................................................... 92
Figure 92: 10% Metakaolin cube .................................................................................... 92
Figure 93: 0% and 10% Metakaolin beams .................................................................... 93
Figure 94: Cubes in water bath ....................................................................................... 93

xi
LIST OF TABLES
Table 1: Physical properties (Patil et al., 2011) .............................................................. 12
Table 2: Chemical composition (Patil et al., 2011) ........................................................ 12
Table 3: Summary of past experiments and optimum metakaolin content ..................... 22
Table 4: K values to determine stone content (The Concrete Institute, 2013) ............... 28
Table 5: Water requirement of concrete mix (The Concrete Institute, 2013) ................. 30
Table 6: Number and dimensions of samples ................................................................. 30
Table 7: Porosiscope evaluation table ............................................................................ 39
Table 8: Final Mix design for 1m3 .................................................................................. 42
Table 9: Actual mix design for required volume of 0.09m3 ........................................... 42
Table 10: Air permeability results .................................................................................. 54
Table 11: Water permeability results .............................................................................. 55
Table 12: Mix design volume required ........................................................................... 71
Table 13: Conceptual mix design per cubic meter ......................................................... 71
Table 14:Conceptual design per mix .............................................................................. 71
Table 15: Actual design per mix ..................................................................................... 71
Table 16: Sieve analysis of fine aggregate ..................................................................... 78
Table 17: Table of fresh concrete properties .................................................................. 78
Table 18: Compression and flexural strengths ............................................................... 78
Table 19: 7 day loading tests .......................................................................................... 79
Table 20: 28 day loading tests ........................................................................................ 79
Table 21: 56 day loading tests ........................................................................................ 79
Table 22: Result deviation from mean ............................................................................ 80
Table 23: Actual vs NPC estimated strengths ................................................................ 80
Table 24: Mass, density and absorption data .................................................................. 81
Table 25: Air/Water permeability data ........................................................................... 82
Table 26: Water sorptivity data ...................................................................................... 83
Table 27: Water sorptivity results ................................................................................... 83

xii
CHAPTER 1: INTRODUCTION
1.1. Research background and significance
1.1.1. Research background

Concrete is primarily one of the predominant and vastly used material in the construction
industry. Worldwide concrete production amounts to approximately 12 billion tonnes
which requires the production of almost 1.6 billion tonnes of cement (Rashad, 2013).
Swamy (1998), mentions that, despite the excellent performance concrete serves, there
are two aspects which have severely degraded its reputation. Namely, the environmental
implications and the durability aspects of the material.

According to Rashad (2013), for every ton of concrete produced, there is approximately
0.8 tonnes of CO2 that is released into the air, thus accounting for 5-8% of global CO2
emissions. With the rapid climate changes due to global warming, the emission of
greenhouse gasses is carefully monitored and various strategies are being implemented
to mitigate this issue. Extensive research on methods to reduce the CO2 emissions from
the production of concrete is currently a major field of interest in the concrete industry.

The Concrete Institute (2013) places a great deal of emphasis on the sustainability of
concrete. The Brundtland report states that development that can sustain the needs of the
current generation without negatively affecting the capability of forthcoming generations
to sustain their needs can be termed sustainable development (Atkinson, 2000). The
sustainability of concrete would need to balance environmental, economic and social
factors which is collectively known as the triple bottom line.

Narmatha and Felixkala (2017) suggests that repair and maintenance of concrete
infrastructure is a major issue which incurs significant expenditure and additional cement
usage. Consequently, concrete structures should be made resilient to ensure a longer life
span, thus minimizing repairs and reconstructions. Extensive research on ways to enhance
the durability of concrete and concrete structures are being executed due to its economic
implications (Basheer et al., 2001).

1
Figure 1: Durability vs Time and expenditure (The Concrete Institute, 2013)

Producing ‘green’ concrete that has poor durability is not sustainable concrete (Day et al.,
2013). As seen in figure 1; when considering the service life of the structure, it may be
cheaper to use initially expensive but durable methods as seen in scenario B and C
compared to initially cheaper methods that need to be rehabilitated and maintained
regularly as seen in scenario A.

1.1.2. Research significance

The main purpose of this research is to identify and investigate alternate materials for
concrete to lower the carbon footprint whilst improving the mechanical properties and the
durability of the material to enable longevity throughout the design life of the structure.
The alternate material (supplementary cementitious material) selected for this research
has been chosen to be metakaolin which is a calcined clay that is readily available.

The cement industry has an enormous impact on the environment and the global warming
contribution due the emissions of greenhouse gasses. Global warming is an important
issue and numerous laws and regulations have been set into motion to reduce the impact
on the environment and to provide sustainable alternatives as a solution/mitigation
measure. There are numerous proposals implemented to measure sustainability which
result in the developments of concepts such as ‘corporate environmental sustainability’
and ‘LEED points systems’ (Atkinson, 2000).

2
Metakaolin which can be used as a supplementary cementitious material; is formed by
the calcination of kaolin clay and is generally very pure and therefore relatively
expensive. Literature has found many advantages of incorporating metakaolin in concrete
(durability, resistance against acid attacks, mechanical properties and resistance to heat
amongst others); however, research into the use of metakaolin in concrete is minimal
(particularly in South Africa). There are significant deficiencies that are seen in scientific
literature on the applications and behavior of this metakaolin used as a binder. The
durability aspects of metakaolin used in concrete can be seen as a major question (Pouhet,
2015).

1.2. Research question


 Is the use of metakaolin a suitable option as a supplementary cementitious
material?
 How does the inclusion of metakaolin influence the properties of concrete?
 What is the optimum metakaolin content to achieve the best durability and
mechanical properties of conventional concrete?

1.3. Research aims


 To investigate the influence of metakaolin on the durability and mechanical
properties of concrete
 To investigate the effect of metakaolin on fresh concrete properties.
 To determine the optimum/critical metakaolin percentage inclusion in concrete
mixes.

1.4. Research objectives


The primary objective of this research is to investigate the influence of metakaolin in
conventional concrete.

 Determine the effect on mechanical properties (7, 28 and 56 day) of varying


metakaolin contents (0%, 5%, 10%, 15%, 20%) in conventional concrete.
 Determine the effect on durability properties (56 day) of varying metakaolin
contents (0%, 5%, 10%, 15%, 20%) in conventional concrete.

3
 Determine the influence of metakaolin on the fresh properties of concrete. This
includes the temperature of the fresh mix, the slump tests and an evaluation of the
finishing of the fresh concrete mix.
 Determine the optimal metakaolin content in conventional concrete by varying
the percentage inclusions of metakaolin.

1.5. Research methodology


 A literature review was done to first acquire knowledge and a background
understanding of the topic of interest. The literature review was used to identify
knowledge gaps, past problems and to develop a method for the research
procedure.
 A conceptual mix design was determined using the relevant data that was
received. The conceptual mix design was then tested and modified to get the actual
mix design that was used. The mixes for 0%,5%,10%,15% and 20% were made
and cast into beams and cubes for testing.
 From the past experiments that were identified from the literature review, the
suitable testing methods for the current research experiments could be determined
and implemented to critically analyze the samples.
 Based on the results acquired from the tests, conclusions and recommendations
can be developed and future research areas can be proposed.

1.6. Dissertation outline


The following section provides an outline of what is to be expected in the subsequent
chapters of this report.

 Chapter 1: Introduction

Rationale is provided on the predicament faced by the concrete and cement industry and
its effect on the environment with global warming particularly. This chapter provides the
background and purpose of this research. The chapter successively identifies the aims and
objectives of this research and presents the research methodology that will be followed
to perform this research.

4
 Chapter 2: Literature review

The literature review continues from the dilemma stated in section 1.1 and follows a
structured and logical process of analyzing literature till a suitable solution is determined.
This chapter starts off by understanding the main properties and impact of conventional
concrete; an enlightenment into supplementary cementitious materials; Metakaolin as a
SCM which delves into the background, physical and chemical properties, processing,
influence on conventional concrete, past research and experiment and finally metakaolin
in South Africa.

 Chapter 3: Methodology

Various methods are identified that will be used to achieve the aim and objectives
stipulated in section 1.3 and 1.4. This chapter will expound on the materials to be utilized,
their properties; the conceptual mix design and how it was determined and the
experimental apparatus and procedures used to determine the concretes fresh properties,
mechanical properties and durability properties.

 Chapter 4: Results and discussion

This chapter presents the results obtained from the experimental procedures that were
used to meet the aims and objectives of this research. The results will be displayed as
summarized graphs and tables and will be followed by a discussion. The initial intricate
data used to obtain the summarized results can be found in appendix B. The chapter will
delve into the outcomes obtained from experimental procedures to determine the material
properties; constituent contents; final mix designs and the results obtained from the
analysis of fresh properties tests, mechanical properties tests and durability tests.

 Chapter 5: Conclusion and recommendations

This chapter provides the final remarks and summarized evaluation of the results and
discussions from chapter 4. A reasonable judgement and recommendation is made for the
use or further research of metakaolin in concrete based on the conclusion of the results
obtained. This chapter also presents areas for future research that can improve the data
and knowledge on the use of metakaolin in concrete.

5
CHAPTER 2: LITERATURE REVIEW
2.1. Introduction
Continuing from section 1.1, the challenge of building sustainable concrete structures
remains the dilemma of the 21st century in the construction industry. Due to the
production of cement, the construction industry has become a primary instrument in its
contribution to climate change, resulting from a high greenhouse gas contribution. The
construction industry must determine not only how they can meet the infrastructural
needs, but also, reduce cement production whilst simultaneously improving the concretes
durability (Mehta and Burrows, 2001).

Mehta and Burrows (2001) compares that the lime-pozzolan concrete structures such as
the 2000 year old Pantheon in Rome, which is still in excellent condition despite the fact
that most modern concrete structures made with Portland cement are rapidly
deteriorating. They further state that most modern structures exposed to corrosive or
marine environments face durability problems within 20 years of casting. Figure 2 shows
the excellent condition of the Pantheon which is the world’s largest unreinforced concrete
dome (The Concrete Institute, 2013); figure 3 and 4 show the deterioration of modern day
structures consisting of a column and bridge respectively.

Figure 2: The Pantheon (Rolling Rome S.R.L, 2014)

6
Figure 3: Deteriorated Figure 4: Deteriorated bridge (Shimomura, 2004)
column (National Research
Council of Canada, 2003)

2.2. Conventional concrete


For the purposes of this literature review, the analysis of conventional concrete will be
omitted due to extensive research being readily available on this aspect. The main
concerns which aid and support the need for the research will be identified.

2.2.1. Environmental concerns

The concrete industry is known to consume enormous amounts of natural resources whilst
releasing harmful greenhouse gasses into the atmosphere as mentioned in section 1.1.
Research into finding alternative materials which can provide durability, strength,
economic advantages, environmental friendliness and sustainability to concrete is of
paramount importance (Cobîrzan et al., 2015).

Hokfors (2014) states that there are two main facets in cement production that are the
contributing factors to the large CO2 emissions. The calcination of lime to cement requires
large amounts of heat and therefore a large amount of energy which use fossil fuels as
their primary source of energy. The use of fossil fuels in this extent results in the release
of CO2 as the byproduct of the combustion reaction required to produce the energy for
the calcination process. Furthermore, additional CO2 is released as a byproduct of the

7
calcination process of the limestone in order to produce cement. This process can be seen
in figure 5. Hokfors (2014) further states that the CO2 released from the combustion
energy and calcination process account for 40% and 60% respectively of the total CO2
emissions released from manufacturing cement.

Figure 5: CO2 emissions from cement production (Hokfors, 2014)

2.2.2. Chemical and Mechanical properties

Concrete can be referred to as a chemically bonded ceramic if it was produced with a


hydraulic cement binder such as Portland cement. Concrete is formed due to the hydration
reaction of the cement which produces a solid and pore system within the concrete. The
pore system has a significant effect on the chemical, mechanical and transportation
properties of concrete (Kumar and Bhattacharjee, 2003). Basheer et al. (2001) states that
concrete’s engineering properties (durability, strength, permeability and shrinkage) are
directly affected by the amount, type, distribution and size of pores in the paste; the
aggregates and its interface between the cement paste.

According to the The Concrete Countertop Institute (2007), the compressive strength of
concrete can be increased by a decrease in calcium hydroxide and a production of more
cementing compounds. Sabir et al. (2001) states that fully hydrated Portland cement
produces approximately 28% of calcium hydroxide which has no significant contribution
to strength and can negatively affect the durability of concrete. This calcium hydroxide
can be eliminated and utilized by adding a pozzolan to react with it to produce calcium
silicate hydrates which will be explained further in section 2.4.5.1.

8
2.2.3. Durability and deterioration

Concrete durability is the most significant property of concrete, as the other properties of
the concrete cannot be displayed if it is unable to accommodate the design life of the
structure. The durability of the concrete will also have a direct effect on the economics as
durable concrete may be more expensive outright but may be far cheaper when
considering the repairs, maintenance and replacement of poor durability concrete over the
design life (Day et al., 2013) which can also be seen in section 1.1.

There are multiple transport mechanisms in concrete; these include diffusion (gas, water
vapour and ionic), absorption and permeability. These transport mechanisms cause the
deterioration of concrete and its durability by the mechanisms seen in figure 6. The most
influential deterioration mechanisms are carbonation, chloride attack, sulphate attack,
corrosion and freeze-thaw. The influence of these mechanisms is greatly influenced by
the number of pores, size of pores, voids and capillaries in the concrete.

Contribution of deterioration mechanisms


Abrasion AAR
Chemical attack Acid attack
Alkali attack Carbonation
Chloride attack Leaching
Salt attack Sulphate attack
Corrosion Cracking
Freeze-thaw

Figure 6: Contribution of deterioration mechanisms (Basheer et al., 1996)

2.3. Supplementary cementitious materials and partial cement replacements


The most essential change from common practice is to acknowledge that improving the
quality and durability of concrete is not only subjected to the influence of the water-binder
ratio. Combining this mindset whilst considering the sustainability and environmental
impacts in the production of cement, draw attention to the use of cement replacement
materials and supplementary cementitious materials (Day et al., 2013).

9
SCM’s are currently being used to decrease the clinker factor in Portland cement and
therefore reduce the CO2 production. These materials are known to significantly enhance
the properties of concrete such as durability, strength and impermeability through
pozzolanic or hydraulic reactions. The main constituent of SCM additives usually consist
of an active amorphous SiO2 (El-Diadamony et al., 2016).

SCM’s can influence the properties of concrete by pozzolanic or hydraulic activity. Some
common SCM’s are fly ash, silica fume, ground granulated blast-furnace slag and
calcined clays. The addition of SCM’s produces concrete that is economical with
increases durability and mechanical properties (Portland Cement Association, 2018).

Figure 7: Supplementary cementitious materials(Portland Cement Association, 2018)

Natural pozzolans are siliceous or siliceous/aluminous materials that need to be mixed


with cement/lime and water in order to form cementing compounds (Cobîrzan et al.,
2015). The Romans were known for founding the concrete industry based on natural
pozzolans and their impressive characteristics can be seen in most roman buildings such
as the Pantheon seen in section 2.1. Despite the impressive history, the use of natural
pozzolans are not being widely utilized in the modern concrete industry (Day et al., 2013).

The main reason for the use of natural pozzolans as a SCM is due to durability
improvements and availability of the raw materials (El-Diadamony et al., 2016).
Industrially produced SCM’s have become less available due to the fact that the rate of
production of concrete exceeds the rate of production of the SCM’s through their

10
industrial processes. However, natural pozzolans such has metakaolin are readily
available as they produced from raw materials such as clay which is in abundance on the
earth’s crust. The use of natural pozzolans as a SCM removes the boundary/limitations
on its availability as they are not controlled by a third party which is producing the SCM
as a secondary product (Mikhailenko, 2012).

2.4. Metakaolin
2.4.1. Background and properties

Metakaolin is an aluminosilicate material formed by the calcination of kaolinite which is


a natural pozzolan. Kaolinite is a hydrous aluminium silicate material formed by the
decomposition of feldspar. The mineral structure contains sheets/layers of aluminium
oxide (hydroxide) sheets weakly bonded with silica sheets as seen in figure 9. The
calcination process removes all water present in the mineral and is thereafter ground to
the required fineness. The calcination process is also known as dehydroxylization which
is the loss of hydroxyl ions. The calcination of kaolinite occurs at a temperature of 700 –
800 degrees Celsius and the calcined product is called metakaolin. (Kalaiyarrasi, 2017).

Figure 8: Kaolinite (Rashad, 2013) Figure 9: Kaolinite Structure (Rashad, 2013)

Equation 1 shows the conversion of kaolin to metakaolin and water (Nita et al., 2004).

700−800°𝐶
𝐴𝑙2 𝑆𝑖2 𝑂5 (𝑂𝐻4 ) → 𝐴𝑙2 𝑂3 . 2𝑆𝑖𝑂2 + 2𝐻2 𝑂 (Eq. 1)

11
Metakaolin contains the silica and alumina that reacts with the calcium hydroxide (by
product of the cement hydration process) in the presence of moisture. The reactivity of
the metakaolin is entirely dependent on the thermal treatment (dehydroxylization of the
kaolin clay) and the grade of clay being utilized (Tironi et al., 2012).

2.4.2. Physical properties of metakaolin

Table 1: Physical properties (Patil et al., 2011)

Specific gravity 2.4 – 2.6


Physical form Powder
Color Off-white, grey to buff
Brightness 80-82 Hunter L
BET 15 m2/g
Specific surface 8-15 m2/g

2.4.3. Chemical composition of metakaolin

Table 2: Chemical composition (Patil et al., 2011)

Silicon dioxide (SiO2) 51 - 53 % Calcium oxide (CaO) < 0.2 %


Aluminium oxide (Al203) 42 - 44% Magnesium oxide (MgO) < 0.1 %
Ferric oxide (Fe2O3) < 2.2 % Sodium oxide (Na2O) < 0.05 %
Titanium oxide (TiO2) < 3.0 % Potassium oxide ()K2O < 0.4 %
Sulphate (SO4) < 0.5 % LOI < 0.5 %
Phosphorus oxide (P2O5) < 0.2 %

2.4.4. Processing of metakaolin and high reactivity metakaolin.

2.4.4.1. Extraction

Kaolinite or kaolin clay is a natural material found in the earth’s crust. These deposits
contain sand which must be separated. The particles of kaolin are very small compared
to sand, therefore, mixing water and chemical dispersants with this deposit would allow
for separation of these particles as they would settle at different rates. The lighter kaolin
particles would be extracted from the upper layer of the fluid medium and collected to
form a wet mix which would then dry and harden (Vancouver, 2002).

12
2.4.4.2. Metakaolin production and calcination

Kaolinite is a hydrated aluminum disilicate, Al2Si2O5(OH)4. The conversion of kaolinite


to metakaolin is done by a process of dehydroxylization, which dehydrates the material
by heat at a temperature of 500° C - 800° C. This process is commonly referred to as
calcination which produces a highly pozzolanic material. Kaolin clays can be calcined in
rotary kilns, fluidized beds or by flash calcination with calcination times as hours ,
minutes, seconds for each calcining method respectively (Vancouver, 2002).

The calcination reaction of kaolinite specified in equation 1, does not produce any CO2
in comparison to the cement production seen in figure 5 located in section 2.2.1. The CO2
emissions produced in the formation of metakaolin are a result of extracting the raw
materials, transportation methods and the production of energy for calcination
(Cassagnabere et al., 2010).

Figure 10: Production of metakaolin by flash calcination (Cassagnabere et al., 2010)

13
2.4.5. Influence of metakaolin on conventional concrete

Metakaolin is a highly reactive pozzolan that performs well when used in conjunction
with fly ash or slag; thus allowing for an increased amount of cement replacement
resulting in green concrete. Benefits such as the improved durability and mechanical
properties result in a prolonged service life which contributes to sustainability and
decreases overall greenhouse gas emissions and expenditure (Whitemud World Cement,
2010).

Siddique and Klaus (2009) states the use of metakaolin in concrete is beneficial for high
strength./high performance concrete, precast concretes, glass fiber and ferro-cement
products, repair mortars and plasters. The benefits of using metakaolin can be seen by the
increase in mechanical properties (compression and flexural strengths), reduction in
permeability, improved durability and resistance to chemical attacks, improved concrete
finishing and reduced efflorescence.

2.4.5.1. Mechanical and durability properties of concrete with metakaolin

Research has shown that metakaolin has positive effects on the strength of concrete which
are dependent on the water/binder ratio and metakaolin quality. The main two reasons
that can be accredited for this effect is the filler effect and the development of calcium-
silicate-hydrates. The filler effect is seen due to the fact that metakaolin is finer than
Portland cement, thus making it capable of getting into the voids and therefore producing
an overall denser concrete with reduced porosity (Zeljkovic, 2009).

Figure 11: The filler effect (Wiggins, 2011)

14
Metakaolin on its own holds no cementing property, however, in the presence of moisture
it will rapidly react with calcium hydroxide to form cementing compounds. The calcium
hydroxide also known as free lime can be seen as by-product in the hydration reaction of
the cement as seen in section 2.2.1.1. The addition of metakaolin to conventional concrete
results in the reaction of the calcium hydroxide (CH) with the alumino-silicate pozzolan
forming additional cementitious compounds; such as calcium-silicate-hydrate (CSH) gel,
and crystalline compounds which include calcium aluminate hydrate and alumino-silicate
hydrates (C2ASH8, C4AH13 and C3AH6). Although this reaction may be slower than plain
Portland cement, the binding properties are significantly improved (El-Diadamony et al.,
2016).

The following quote has been taken from Patil et al. (2011). The quoted text shows that
the inclusion of metakaolin in concrete utilizes the non-cementitious compounds that
were formed as a by-product of the hydration reaction of cement and converts them into
cementitious compounds.

“Cement + water = Calcium Silicate (Cementitious)

+ Calcium Hydroxide (Non-cementitious)

Calcium Hydroxide + Metakaolin = Calcium Aluminate (Cementitious)

+ Calcium Alumino Silicate (Cementitious)”

Figure 12: Calcium hydroxide content for metakaolin replacement (Sabir et al., 2001)

15
The calcium hydroxide by-product is seen as an infuriation in the construction industry
as it compromises the durability properties of the concrete (Anbarasan and Venkatesan,
2015). The calcium hydroxide by-product has little to no beneficial contribution to the
concrete strength. The inclusion of metakaolin enables a pozzolanic reaction with the
calcium hydroxide in the presence of moisture to produce additional cementing properties
(Aiswarya et al., 2013).

Large percentage contents of metakaolin show reduced early strengths due to the dilution
effect. The dilution effect is a result of the reduced cement content in the concrete mix
which decreases the hydration reaction. This decrease further results in a lower
production of the calcium hydroxide required for the pozzolanic reaction of metakaolin,
thus causing what is known as the dilution effect (Abdul Razak and Wong, 2005).

The mechanical and durability properties of concrete is improved by the ability of


metakaolin to increase the density and packing; decrease the number and size of pores;
and reduce the permeability of concrete (Whitemud World Cement, 2010). Whitemud
World Cement (2010) indicates that concrete with the addition of metakaolin results in
an increase in the compressive strength and an increase in durability properties as seen in
figure 13 and 14 respectively.

Figure 13: Metakaolin compressive strength Figure 14: Metakaolin ASR mitigation
(Whitemud World Cement, 2010) (Whitemud World Cement, 2010)

16
2.4.5.2. Rheology and fresh concrete properties

Al Menhosh et al. (2016) showed that the setting time of concrete decreased with
increased metakaolin contents displaying accelerator properties. The research also
showed that the workability decreased with higher metakaolin contents and increased
with higher water-binder ratios. Compression and flexural strengths increase and the
water absorption is seen to decrease with the higher metakaolin contents.

Ambroise et al. (1994) states that there is a low dispersion ability of metakaolin in
concrete mixes due to the fineness of the particles. Further research is being conducted to
mitigate this issue and reduce the water demand or use of super plasticizers for concrete
with metakaolin.

Figure 15: Slump comparison (Wiggins, 2011)

Abdul Razak and Wong (2005) states that the rate of hydration is a function of
temperature, therefore suggesting that the development in strength is dependent on the
time-temperature history (considering sufficient moisture available for hydration).

The use of metakaolin reduces bleeding of the fresh concrete due to the fineness of the
metakaolin particles which restrict capillary channels minimizing the rise of fresh water
to the surface and the settlement of the aggregate. Concrete with metakaolin has a
tendency to exhibit a creamy texture, which allows for better finishing and would also
result in improved pumpability (Biju and H, 2016).

17
2.4.5.3. Environmental aspects

Whitemud World Cement (2010) states that the production of metakaolin requires a
temperature of 800° C which is almost half of 1500° C which is required to produce
Portland cement. The reduced greenhouse gas emissions can be attributed to the fact that
there are no CO2 emissions as a by-product from the calcination reaction of metakaolin.
The reduced energy usage and lack of CO2 emissions from the reaction results in a
minimum of 55% decrease in greenhouse gas emissions.

Figure 16: Metakaolin CO2 footprint (Whitemud World Cement, May 2010)

Cassagnabere et al. (2010) states that for 1 ton of flash metakaolin produced,
approximately 175 kg of CO2 is released into the atmosphere; compared to approximately
1 ton of CO2 emissions released for every ton of Portland cement. Due to the fact that
metakaolin contains a high percentage of aluminosilicates, allowing it to maximise the
amount of durable binders in concrete as it produced a rapid aggressive reaction with lime
compared to fly ash which may take almost two months to react with the lime in concrete.
The use of metakaolin significantly prolongs the life of the concrete and the reduction in
rebuilding/replacing concrete is the fundamental option in order to conserve resources
and reduce greenhouse gas emissions.
18
2.4.5.4. Economic and social aspects

Figure 17 shows the estimated costs when replacing Portland cement with 25% fly ash
and 5% metakaolin. The costing shows that the inclusion of metakaolin despite being
more expensive than concrete resulted in cheaper mix design due to the inclusion of an
additional supplementary cementitious material (fly-ash) which is cheaper than cement.
The combined benefit of the cheaper but weaker properties of fly-ash with the expensive
but stronger properties of metakaolin resulted in an overall improvement to the strength,
durability and the economic analysis of the concrete (Vancouver, 2002).

Figure 17: Concrete production costs (Vancouver, 2002)

Abdul Razak and Wong (2005) states that one of the most influential factors on the
profitability of a construction project is the speed of construction. Such as reducing
standing time of formwork due to reduced curing times of concrete to achieve the target
strengths. The use of metakaolin is seen as an accelerator which decreases the setting time
of concrete and is also able to increase the strengths of concrete resulting in greater early
strengths therefore increasing the speed of construction.

19
2.4.6. Past research

Badogiannis and Tsivilis (2009) studied the pore structure of the concrete using mercury
intrusion porosimetry. Concrete with metakaolin displayed reduced gas permeability
values compared to that of conventional concrete. The increase of metakaolin exhibited
a relative decrease in the concrete sorptivity values. The inclusion of metakaolin in
concrete was found to decrease the overall porosity and mean pore size of the concrete
thus making it more durable against transportation mechanisms that may deteriorate
concrete.

Güneyisi et al. (2007) concluded that high strength and low shrinkage concretes can be
obtained by the inclusion of ultra-fine metakaolin. The inclusion of metakaolin resulted
in an increase in both compression and splitting tests. The dominating factor influencing
shrinkage was found to be the water/cement ratio rather than the content of metakaolin.
Using metakaolin as a partial cement replacement improved the pore structure and pore
size distribution, decreasing the total porosity of the concrete.

Gruber et al. (2001) tested the effects of high-reactivity metakaolin (HRM) in concrete
and found that the use of 8% and 12% HRM greatly decreased the coefficient of chloride
ion diffusion by 50% and 60% respectively. This kind of results can be expected to extend
the service life of a structure in chloride environments. Partial replacement of 20% HRM
greatly reduced the pore solution alkalinity below that required for alkali-silica reactivity
but above the pH necessary to ensure steel passivation.

Siddique and Klaus (2009) suggests that metakaolin alters the pore structure of concrete
and decreases the permeability which is responsible for the transportation of water and
diffusion of ions which lead to its deterioration. The experiments conducted show that
10% and 15% metakaolin replacements enhanced durability to sulphate attack. It is
further suggested that 10% and 15% high reactivity metakaolin contents may be suitable
to control deleterious expansion from alkali-silica reactions in the concrete.

20
Jian-Tong and Zongjin (2002) compared metakaolin against silica fume on the influence
of strength, workability, shrinkage and resistance to chloride attack. It was found that
metakaolin had better workability than silica fume. The strength and shrinkage of the two
material replacements were similar whilst the silica fume performed better in chloride
diffusion.

Bai et al. (2000) reveals that cement replacement up to 15% of metakaolin results in
substantial strength improvements for water-binder ratios between 0.4 and 0.6. It was
found that the increase in metakaolin content significantly decreases the setting times of
the concrete mixes (Al Menhosh et al., 2016). However, some research indicate that the
inclusion of metakaolin has a retarding effect on the concrete setting times (Sabir et al.,
2001). Bai et al. (1999) concludes that the use of metakaolin in concrete significantly
reduces the workability and slump of the concrete and the use of superplasticizers are
essential. The use of superplasticizers results in improved dispersal of the metakaolin
particles credited to the thixotropic behavior of the metakaolin and reduced voids.

Aiswarya et al. (2013) concludes that metakaolin is an effective SCM and generally
requires more super plasticizers compared to conventional concrete. It is further
suggested that the use of metakaolin may be uneconomical due to its high costs but may
be economical when considering durability and strength aspects.

Abdul Razak et al. (2004) states that curing methods have a significant influence on the
properties of concrete. Full water curing resulted in the least permeable concrete with air
dried concrete exhibiting inferior durability characteristics near the surfaces. The research
compared conventional concrete to metakaolin and to silica fume inclusions. The results
showed that the inclusion of these supplementary materials decreased the surface
absorption, water absorption and water sorptivity of the concrete. However, the
improvement was found to be marginal after 28 days indicating the completion of the
pozzolanic reaction.

21
Extensive research performed by Dhinakaran et al. (2012) reports that by increasing
metakaolin contents the following can be observed; a reduction in workability; an
increase in compressive and flexural strengths; greater resistance to chloride penetration;
minor reductions in the pH value which is insignificant. The research also suggests that
metakaolin showed a greater percentage increase in strength with higher water-binder
ratios.

Table 3: Summary of past experiments and optimum metakaolin content

Author Metakaolin % W/C ratio Optimum Comments


(Dhinakaran 5%, 10%, 15% 0.32 15% Suggests the
et al., 2012) 0.35 10% metakaolin benefits are
0.40 10% greater at higher
0.50 10% water/binder ratios
(Ženíšek et 0%-25% 0.3 -0.241 10% Water/binder ratio
al., 2016) varied with varying
metakaolin contents
(Dinakar et 5%, 10%, 15% 0.3 10%
al., 2013)
(Dubey and 5%, 10%, 15% 0.5 10%
Chandak,
2015)
(Weng et al., 0%-25% 0.5 15% Efflorescence of
2013) concrete reduced with
0-15% metakaolin
(Jagtap et al., 0%-25% 0.42 15% Workability decreases
2017) with an increase in
metakaolin
(Wong and 0%-15% 0.27 10 &15% The compressive
Abdul Razak, strengths for 0.27 and
2005) 0.3 10 & 15% 0.33 showed optimum
metakaolin content of
0.33 10% 15 and 10% for 28 and
180 days respectively.
(Subbamma 0%-20% - 15% Used with varying
and Reddy, contents of fly ash (0-
2016) 30%)
(Güneyisi et 0%, 10%, 20% 0.35 20%
al., 2007) 0.55 20%
(Patil and 0%, 7.5%, 0.31 7.5%
Kumbhar, 10%, 12%,
2012) 15%
(Kaur and 0%, 3%, 6%, 0.4 9%
Sran, 2016) 9%, 12%
(Biju and H, 2.5%, 5%, 0.3 10% 70MPa mix design and
2016) 7.5%, 10%, the use of
12.5% superplasticizers

22
The most relative literature that can be reviewed is the study conducted by Bakera and
Alexander (2018), which investigated the properties of concrete containing metakaolin as
a supplementary cementitious materials in the Western Cape (South Africa). This study
also used the same metakaolin supplied by the Kaolin Group.

The study done by Bakera and Alexander (2018) assessed the influence of metakaolin on
the durability and mechanical properties of concrete. The study tested varying metakaolin
contents at varying water-binder ratios. The study tested 0%, 5%, 10%, 15% and 20%
inclusions of metakaolin; for 0.4, 0.5 and 0.6 water-binder ratios. The compressive
strengths decreased with increasing water-binder ratios and all the inclusions of
metakaolin showed higher strengths than the control mix. The results showed that the
increase in the metakaolin increased the compressive strength of the concrete. The tensile
splitting test showed similarity to the compression tests and the same trend that the
increase in metakaolin contents increased the tensile strength of the concrete was found
to be true. The use of this high reactivity, flash calcined metakaolin resulted in a general
increase with the increasing metakaolin contents and was unable to provide a definite
optimal metakaolin content due to the percentage range used. The optimal percentage
inclusion of metakaolin therefore stated 20% addition of metakaolin as the optimal
percentage inclusion.

Bakera and Alexander (2018) also tested the elastic modulus on the samples and found
that the elastic modulus decreased with the increasing water-binder ratios. The elastic
modulus increased with the use of metakaolin. Durability tests such as oxygen
permeability index, water sorptivity index and chloride conductivity index all showed an
overall increase in all durability aspects due to the inclusion of metakaolin. The 0.6 water-
binder ratio showed a decrease in permeability which could be associated with the
allowance of pozzolanic reactions due to sufficient space to accommodate the reactions.
However, the 0.4 water-binder ratio showed the greatest reduction which can be attributed
to the low formation of capillary pores during the hydration.

23
2.4.7. Metakaolin in South Africa

Ekosse (2010) indicates that the occurrence of kaolin deposits in the southern part of
Africa prevail over other regions in Africa (figure 18). South Africa in particular
dominates in terms of number of kaolin deposits compared to the southern region as
shown in figures 19. The research further states although majority of the deposits are
easily accessible and occur in large quantities, the exploitation of this valuable resource
in African industries are relatively low. Ekosse (2010) concludes that there is a solid
economic potential for the kaolin market in Africa and recommends that this market be
developed. Kaolin is mined on the surface and is environmentally friendly as the old
mines can be easily reclaimed and fully rehabilitated.

Figure 18: Kaolin deposits in Africa (Ekosse, 2010)

Figure 19: Kaolin deposits in Southern Africa (Ekosse, 2010)

24
2.5. Chapter summary
2.5.1. Mechanical properties

The addition of metakaolin in concrete is seen to significantly increase the mechanical


properties of concrete. Mechanical properties such as compression strength, flexural
strength and tensile strength increase with an increase in the metakaolin content until the
optimum and the decrease, however, all additions of metakaolin are seen to be stronger
than the ordinary Portland cement concrete.

2.5.2. Durability

The durability of the concrete is drastically increased with the inclusion of metakaolin as
it reduces pores and their sizes in the concrete also resulting in a much denser mix. This
reduction in pores has a direct effect of the transportation mechanisms and therefore is
capable of resisting degradation much better than ordinary concrete. The durability of
samples were tested by oxygen permeability indexing, water sorptivity, chloride
conductivity, mercury intrusion porosimetry and SEM imaging amongst others.

2.5.3. Rheology and workability

Due to the fineness of metakaolin being finer than cement, the metakaolin content has a
much greater surface area and therefore requires more water for dispersion in the
concrete. The overall effects can be seen that the inclusion of metakaolin reduces the
workability of the mix and produces lower slumps. Metakaolin is found to accelerate the
setting time of concrete and provide enhanced finishing properties.

2.5.4. Water requirement.

Research showed that the addition of metakaolin showed greater percentage increases in
the mechanical and durability properties of concrete mixes with higher cement-binder
ratios. As mentioned in section 2.5.3, the inclusion of metakaolin substantially reduced
the slump of the concrete and therefore requires large amounts of water or a
superplasticizer for dispersion of the metakaolin. The use of a superplasticizer is highly
recommended.

25
2.5.5. Finishing

The use of metakaolin which is a white powder results in a lighter colour concrete. The
use of metakaolin is also seen to reduce the efflorescence of concrete, thus making it
suitable for coloured concrete (Day et al., 2013). Evidence of the lighter colour of the
concrete with metakaolin can be seen in appendix C.

2.5.6. Experimental methods

From the review done on past research and experiments the following experiments/testing
procedures have been selected to be suitable to the current research topic of investigating
the use of metakaolin in concrete. The following experimental methods have been used
in past experimental investigations of a similar nature.

Mechanical properties:

 Compressive strength.
 Flexural strength.
 Tensile splitting strength.
 Elastic modulus tests.

Durability Properties:

 Oxygen permeability index and Chloride conductivity tests.


 Carbonation and Alkali-Silica reactivity
 Sulphate and acid attack.
 Water penetration and Water sorptivity.
 Abrasion and shrinkage tests.
 Freeze-thaw and fire exposure tests.
 X-Ray diffraction
 Microscopy analysis (Scanning electron microscope)

However, the experiments that could be performed were restricted to the availability of
the testing equipment to the students. The experiments that were possible for this research
will be identified and elucidated in chapter 3.

26
CHAPTER 3: METHODOLOGY
3.1. Introduction
The following chapter identifies the various methods that will be used in order to achieve
the aim and objectives stipulated in section 1.3 and 1.4. This chapter will elucidate the
materials to be utilized, their properties; the conceptual mix design and how it was
determined and the experimental apparatus and procedures used to determine the
concretes fresh properties, mechanical properties and durability properties. The test
methods are done in accordance to SANS/SABS standards. Where there were limitations
in the testing according to the standards, the tests were performed as close as possible to
the standards.

3.2. Materials and their properties


3.2.1. Cement

NPC original black CEM II/B-S 42.5 N PLUS was selected to be used for the concrete
mix as this as the cement that was provided by the university. This cement manufacture
was chosen considering the fact that existing data regarding the water-binder ratios and
relation to the 28-day strengths were provided by NPC. This graph can be seen in the
appendix as figure 54.

3.2.2. Fine aggregate

Umgeni river sand will be used as the fine aggregate. This sand has a relative density of
2.65. The fineness modulus of the fine aggregate was determined by sieve analysis done
in accordance to SANS 201.

Sieve analysis to determine fineness modulus:

Apparatus:

 500g of dried fine aggregate.


 Sieves (4.75mm, 2.36mm, 1.18mm, 0.6mm, 0.3mm, 0.15mm, pan)
 Vibrating machine and cleaning tools.
 Weighing scale.

27
Method:

A 500g sample of the fine aggregate was dried in the oven for 24 hours to remove
moisture. The sieves are stacked from smallest to largest openings and the sample is
poured through the top. The sieves are then placed in the vibrator for 2 minutes. The sand
retained on each sieve is then removed, weighed and recorded in the table as seen in the
appendix B. The formula seen in equation 2 is then used to calculate the fineness modulus.

Σ 𝑜𝑓 𝑐𝑢𝑚𝑢𝑙𝑎𝑡𝑖𝑣𝑒 𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑟𝑒𝑡𝑎𝑖𝑛𝑒𝑑


𝐹𝑀 = (𝐸𝑞. 2)
100

Figure 20: Specified sieves Figure 21: Vibrating machine

3.2.3. Coarse aggregate

Tillite stone will be used as the coarse aggregate. The stone has a relative density of 2.65
and a compacted bulk density of 1446 kg/m3 which was tested and stated by the aggregate
provider. Table 4, obtained from the Fundamentals of concrete textbook (The Concrete
Institute, 2013) and equation 5 will be used to determine the stone content for the mix.

Table 4: K values to determine stone content (The Concrete Institute, 2013)

Approx. slump Compaction K


range (mm) Nominal maximum size of stone (mm)
9.5 13.2 19.0 26.5
75-150 Hand compaction 0.75 0.84 0.94 1
25-100 Moderate vibration 0.8 0.9 1 1.06
0-25 Heavy vibration 1 1.05 1.08 1.10

28
3.2.4. Metakaolin

Metakaolin KG-K40 (high reactivity, flash-calcined metakaolin) which was sponsored by


the Kaolin-Group will be used as the supplementary cementitious material. Figure 22
shows the chemical and physical analysis of the metakaolin that will be used in the
concrete mix.

Figure 22: Metakaolin KG-K40 analysis (Kaolin-Group, 2018)

Figure 23: High reactivity KG K40 Metakaolin

29
3.2.5. Water

The water-cement ratio will be termed as the water-binder ratio, since the binder will
consist of cement and metakaolin. The water-binder ratio is the proportion of the mass of
binder to the mass of fresh water that will be used in the mix. The moisture absorption
properties of the admixture, dry aggregates, mixing drum and apparatus was not taken
into consideration due to the time limitation given to this research.

The water-binder ratio is inversely proportional to the strength of the mix and directly
proportional to the permeability of the mix. A suitable water-cement ratio for
conventional concrete ranges from 0.45-0.8 (The Concrete Institute, 2013). Table 5 is
taken from the Fundamentals of concrete textbook (The Concrete Institute, 2013). The
table suggests the following water requirements for concrete mixes without admixtures
to provide a 75mm slump.

Table 5: Water requirement of concrete mix (The Concrete Institute, 2013)

Nominal size of stone (mm) Water requirement of concrete (l/m3)


9.5 235
13.2 225
19 210
26.5 200
37.5 190

3.2.6. Moulds for concrete samples

The following dimensions for the moulds are in accordance to SANS 5860. An additional
cube was made per sample for durability tests. An addition of 15% for wastage was added
when determining required volume of mix (presented in section A.2 in appendix A).

Table 6: Number and dimensions of samples

Number Sample Dimension Volume Number of Number of


per mix (mm) (m3) mixes testing
per testing days
days
3 Cube 150 x 150 x 150 0.3375 5 3
3 Beam 100 x 100 x 500 0.045 5 3

30
3.3. Conceptual mix design
The mix design was calculated using the C&CI method (Cement and Concrete Institute)
which is based on the ACI (American Concrete Institute) standard 211.1-91 (The
Concrete Institute, 2013).

Method:

 Identify materials to be used and their properties and characteristics such as


relative densities, compacted bulk densities, fineness modulus and maximum
stone size.
 Determine the required concrete strength and slump from the graph in appendix
A - figure 54 which was supplied by NPC. This can then be used to determine the
required water-binder ratio.
 The water requirement was determined from Table 11.4 from the Fundamentals
of concrete textbook (The Concrete Institute, 2013) which is displayed in table 5.
 The cement content was calculated using the following formulas.

𝑤𝑎𝑡𝑒𝑟
= 𝑊𝐶 𝑅𝑎𝑡𝑖𝑜 (𝐸𝑞. 3)
𝑐𝑒𝑚𝑒𝑛𝑡
𝑤𝑎𝑡𝑒𝑟
𝑐𝑒𝑚𝑒𝑛𝑡 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 = (𝐸𝑞. 4)
𝑊𝐶 𝑅𝑎𝑡𝑖𝑜

 The stone content was calculated as follows.

𝑠𝑡𝑜𝑛𝑒 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 = 𝐶𝐵𝐷(𝐾 − 0.1 × 𝐹𝑀) (𝐸𝑞. 5)

𝑤ℎ𝑒𝑟𝑒 𝐶𝐵𝐷 = 𝐶𝑜𝑚𝑝𝑎𝑐𝑡𝑒𝑑 𝑏𝑢𝑙𝑘 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 𝑖𝑛 𝑎𝑐𝑐𝑜𝑟𝑑𝑎𝑛𝑐𝑒 𝑡𝑜 𝑆𝐴𝑁𝑆 5845,

𝐹𝑀 = 𝐹𝑖𝑛𝑒𝑛𝑒𝑠𝑠 𝑚𝑜𝑑𝑢𝑙𝑢𝑠 𝑜𝑓 𝑓𝑖𝑛𝑒 𝑎𝑔𝑔𝑟𝑒𝑔𝑎𝑡𝑒,

𝐾 = 𝑓𝑎𝑐𝑡𝑜𝑟 𝑑𝑒𝑡𝑒𝑟𝑚𝑖𝑛𝑒𝑑 𝑓𝑟𝑜𝑚 𝑡𝑎𝑏𝑙𝑒 4

 The sand content was calculated as follows and determined for a 1m3 mix.

𝑐𝑒𝑚𝑒𝑛𝑡 𝑐𝑜𝑛𝑡𝑒𝑛𝑡
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑐𝑒𝑚𝑒𝑛𝑡 = (𝐸𝑞. 6)
𝑐𝑒𝑚𝑒𝑛𝑡 𝑑𝑒𝑛𝑠𝑖𝑡𝑦

𝑠𝑡𝑜𝑛𝑒 𝑐𝑜𝑛𝑡𝑒𝑛𝑡
𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑠𝑡𝑜𝑛𝑒 = (𝐸𝑞. 7)
𝑠𝑡𝑜𝑛𝑒 𝑑𝑒𝑛𝑠𝑖𝑡𝑦

∴ 𝑣𝑜𝑙 𝑜𝑓 𝑠𝑎𝑛𝑑 = 1000 − 𝑠𝑡𝑜𝑛𝑒 𝑣𝑜𝑙. −𝑤𝑎𝑡𝑒𝑟 𝑣𝑜𝑙. −𝑐𝑒𝑚𝑒𝑛𝑡 𝑣𝑜𝑙. (𝐸𝑞. 8)

31
𝑠𝑎𝑛𝑑 𝑣𝑜𝑙.∗ 𝑠𝑎𝑛𝑑 𝑑𝑒𝑛𝑠𝑖𝑡𝑦
𝑠𝑎𝑛𝑑 𝑐𝑜𝑛𝑡𝑒𝑛𝑡 = (𝐸𝑞. 9)
1 𝑚3

 Calculate the volume of concrete required for the mould and account for a 15%
wastage. Use this final volume to factor the material requirements from a 1m3
mix to the desired volume.
 The conceptual mix design can be seen in appendix A, section A.2.

3.4. Mixing and preparation of samples


3.4.1. Mixing the concrete

Apparatus:

 Weighing scale.
 Buckets, shovels, spades and wheelbarrow.
 Tilting drum mixer.
 Moulds
 Vibrating table.
 Curing room with water baths.

Method:

 Conduct the trial mix using the conceptual design. Start by adding all the dry
materials and mixing in the mixing drum for 30 seconds. Add the specified water
to the mix and allow to mix for at least 2 minutes.
 Assess the slump and cohesiveness. Accept, reject or modify the mix to achieve
the target requirements.
 Once the mix is acceptable, pour it into the moulds and place them on the vibrating
table for no longer than 2 minutes.
 Allow the concrete to harden in the moulds for 24 hours, thereafter, carefully
demold the samples and place them in the water baths in the curing room until
required for testing.

32
3.4.2. Workability – Slump test

The slump test was performed in accordance to SANS 5862-1.

Apparatus:

 300mm high conical mould (100mm at top and 200mm at the base).
 Level base plate, measuring ruler and shovel.
 Tamping rod (16mm diameter and a length of 600mm +/- 2mm).

Method:

 Clean the inside surface of the mould with a damp cloth and place it on the base
plate. Fill concrete into the mould in three equal layers, tamping each layer 25
times (distributed evenly throughout the layer without penetrating the previous
layer) with the tamping rod.
 Fill the mould to the top and level it off, thereafter carefully remove the mould off
the base plate. Invert the mould and place it next to the slumped concrete.
 Place the tamping rod horizontally across the top rim of the mould over the
slumped concrete and using the ruler, measure the slump (the highest point of the
slumped concrete to the underside of the tamping rod) and record the result.

Figure 24: Slump test (Big Pics, 2018)

33
3.5. Experimental testing
3.5.1. Mechanical properties - Compression test

The compressive strength test using cubes were done in accordance with SANS 5860,
5861 and 5863. The dimensions used for the cubes are 150mm x150mm x 150mm.

Apparatus:

 Testing machine for compression.


 Cube of specified dimensions.

Method:

 The cube samples were removed from the curing tanks to be tested while
saturated.
 The sample was placed into the testing machine with the smooth faces
perpendicular to the loading and the cast-exposed face parallel to the loading.
 The loading at failure was then recorded and the compression strength was
calculated by the following equation.

𝑃
𝑓𝑐 = (𝐸𝑞. 10)
𝐴

𝑓𝑐 = 𝐶𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑜𝑛 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ ; 𝑃 = 𝐿𝑜𝑎𝑑 𝑎𝑡 𝑓𝑎𝑖𝑙𝑢𝑟𝑒 ; 𝐴 = 𝐶𝑟𝑜𝑠𝑠 𝑠𝑒𝑐𝑡𝑖𝑜𝑛𝑎𝑙 𝑎𝑟𝑒𝑎

Figure 25: Cube in compression test

34
3.5.2. Mechanical properties - Flexural tests

The flexural strength test using beams were done in accordance with SANS 5860, 5861
and 5864. The dimensions used for the beam specimen is 100mm x 100mm x 500mm.
The beam will be supported by two rollers spaced at 300mm and the load will be applied
by two rollers spaced at 100mm apart as shown in figure 26.

Figure 26: Flexural strength test (SANS, 2006)

Apparatus:

 Loading machine with rollers set up as specified in figure 26.


 Beam of specified dimensions.

Method:

 The beam samples were removed from the curing tanks to be tested while
saturated.
 The sample was placed into the testing machine with the smooth faces
perpendicular to the loading and the cast-exposed face parallel to the loading.
 The loading at failure was then recorded and the flexural strength was calculated
by the following equation.
𝑃𝐿
𝑓𝑓 = (𝐸𝑞. 11)
𝑏𝑑 2

𝑓𝑓 = 𝐹𝑙𝑒𝑥𝑢𝑟𝑎𝑙 𝑠𝑡𝑟𝑒𝑛𝑔𝑡ℎ ; 𝑃 = 𝐿𝑜𝑎𝑑 𝑎𝑡 𝑓𝑎𝑖𝑙𝑢𝑟𝑒

𝐿 = 𝐷𝑖𝑠𝑡𝑎𝑛𝑐𝑒 𝑏𝑒𝑡𝑤𝑒𝑒𝑛 𝑠𝑢𝑝𝑝𝑜𝑟𝑡𝑠; 𝐵 = 𝑊𝑖𝑑𝑡ℎ 𝑜𝑓 𝑏𝑒𝑎𝑚; 𝐷 = 𝑑𝑒𝑝𝑡ℎ 𝑜𝑓 𝑏𝑒𝑎𝑚

35
Figure 27: Beam in the flexural strength test

3.5.3. Durability – Density, Water Absorption and sorptivity

The density and water absorption of the cube samples were determined by taking the
average saturated and unsaturated (air dried for 7 days) weights of the samples.

𝑀𝑎𝑠𝑠
𝐷𝑒𝑛𝑠𝑖𝑡𝑦 = 𝑘𝑔/𝑚3 (𝐸𝑞. 12)
𝑉𝑜𝑙𝑢𝑚𝑒

The water sorptivity was done by coring the cube and cutting them into disks, thereafter
placing them in a calcium hydroxide solution and weighing them as stipulated time
intervals.

Apparatus:

 Coring and sawing machine


 Trays, paper towels and plastic rods.
 Calcium hydroxide solution and water.
 Scales and an oven.
 Stopwatch/timer.

36
Method:

 Core a 70mm diameter +/- 2mm core from the cube sample and coat the cored
surface with epoxy and allow to dry. Thereafter, cut four 30mm +- 2 mm thickness
of discs from the core; mark and place them in an oven at 50 degrees celsius for 7
days. Afterward, place them in room temperature and allow them to cool.
 Place the plastic rods in the tray at appropriate distances suitable to support the
specimens. Mix the 3g of calcium hydroxide with 1 litre of tap water and pour
into the tray ensuring that the solution level is at least 2 mm above the rods.
 Weigh the dry mass of the samples and record it.
 Start the timer as soon as you place the specimens on the plastic rods in the
solution.
 At 3, 5, 7, 9, 12, 16,20 and 25 minutes without stopping the timer at each interval;
remove the sample from the solution, wipe the surface of the sample with a paper
towel, weigh and record the mass and the place it back into the solution. Limit the
time of this process to 10 seconds per sample.
 The results were then recorded into excel and the sorptivity calculations were
performed by the following equation.
𝐹∗𝑑
𝑆 = 𝑚𝑚/√ℎ𝑟 (𝐸𝑞. 13)
𝑀𝑠𝑣 − 𝑀𝑠0

𝑤ℎ𝑒𝑟𝑒 𝐹 = 𝑠𝑙𝑜𝑝𝑒 𝑜𝑓 𝑡𝑟𝑒𝑛𝑑𝑙𝑖𝑛𝑒 𝑤𝑖𝑡ℎ 𝑅 2 > 0.98 𝑜𝑓 𝑐ℎ𝑎𝑛𝑔𝑒 𝑖𝑛 𝑚𝑎𝑠𝑠 𝑣𝑠 √ℎ𝑟

𝑑 = 𝑚𝑒𝑎𝑛 𝑠𝑝𝑒𝑐𝑖𝑚𝑒𝑛 𝑡ℎ𝑖𝑐𝑘𝑛𝑒𝑠𝑠 (𝑛𝑒𝑎𝑟𝑒𝑠𝑡 𝑡𝑜 0.02𝑚𝑚)

𝑀𝑠𝑣 = 𝑣𝑎𝑐𝑢𝑢𝑚 𝑠𝑎𝑡𝑢𝑟𝑎𝑡𝑒𝑑 𝑚𝑎𝑠𝑠 (𝑛𝑒𝑎𝑟𝑒𝑠𝑡 𝑡𝑜 0.01𝑔)

𝑀𝑠0 = 𝑜𝑣𝑒𝑛 𝑑𝑟𝑖𝑒𝑑 𝑚𝑎𝑠 𝑜𝑓 𝑠𝑝𝑒𝑐𝑖𝑚𝑒𝑛(𝑛𝑒𝑎𝑟𝑒𝑠𝑡 𝑡𝑜 0.01𝑔)

Figure 28: Cored sample Figure 29: Water sorptivity setup

37
3.5.4. Durability – Air/Water permeability

The air and water permeability tests were done with the assistance of Naidu Consulting
and the use of a porosiscope as specified.

Apparatus:

 C-P-6000 Porosiscope kit (James Instruments)


 Distilled water and lubricant (Vaseline)
 Masonry drill and bit

Method:

 Using a masonry drill, drill 10mm diameter by 40mm deep test holes in the
sample.
 Blow the holes with air to clean and remove dust from the hole.
 Add lubricant to the silicone plug and insert it into the hole with aid of the plastic
screw ensuring a tight seal can be obtained.
 Insert the hypodermic needle into the hole through the center of the plastic screw
 To test the Air permeability, connect the relevant apparatus as specified in the
Porosiscope operation manual and then turn the machine on.
 Use the pump to create a vacuum with a pressure lower than -55kPa which will
be signaled by both LED lights being lit.
 Close the vacuum valve on the machine and wait for the vacuum pressure to rise
to -55kPa. When this happens, the first LED will turn off and the timer will start.
 When the pressure rises to -50kPa, the second LED will turn off and the timer will
stop. Note the time and convert into seconds.
 Use the time obtained from the test in equation 14 to determine the Air Exclusion
Rating (AER).

𝑡 𝑡
𝐴𝐸𝑅 = 19.05 (𝐸𝑞. 14)
55𝑉 52.5 𝑉
( − 𝑣) ( 100 )
50

𝑤ℎ𝑒𝑟𝑒 𝑡 = 𝑡𝑖𝑚𝑒 𝑖𝑛 𝑠𝑒𝑐𝑜𝑛𝑑𝑠; 𝑉 = 𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑎𝑝𝑝𝑎𝑟𝑎𝑡𝑢𝑠 𝑎𝑛𝑑 𝑡𝑒𝑠𝑡 ℎ𝑜𝑙𝑒 (77.1𝑚𝑙)

𝑇ℎ𝑒𝑟𝑒𝑓𝑜𝑟𝑒 𝐴𝐸𝑅 = 0.247 𝑡

38
 To test water permeability, clear the pressure in the apparatus from the air
permeability test and connect the water apparatus as specified by the operation
manual for the Porosiscope.
 Fill the syringe with distilled or tap water and attach it to the machine. Gently
depress the syringe plunger until the water emerges from the overflow tube.
 Adjust the meniscus position to be as close to the outside of the machine by
applying pressure using the syringe plunger and then close the stopcock.
 Both LED lights should be lit and once the meniscus passes sensor one, the first
LED will go off and the timer will start running.
 Once the meniscus passes sensor two, the second LED will go off and the timer
will stop. Note the timer reading and convert it into seconds.
 The Water Absorption Rate is given by equation 15.

𝑊𝐴𝑅 = 100𝑡 𝑠𝑒𝑐𝑠/𝑚𝑙 (𝐸𝑞. 15)

 The porosiscope results are evaluated using table 7.

Table 7: Porosiscope evaluation table

Category Protective Quality Air Permeability Water


Time (s) AER (s/ml) WAR (103/ml)
0 Poor < 30 <8 <3
1 Not very good 30 - 100 8 – 25 3 – 10
2 Fair 100 - 300 25 – 75 10 – 30
3 Good 300 - 1000 75 – 250 30 – 100
4 Excellent > 1000 > 250 > 100

Figure 30: Air permeability Figure 31: Water permeability

39
3.5.5. Scanning Electron Microscope (SEM)

The SEM analysis was done at the Westville campus of UKZN. The samples were tested
after the 28-day curing period. A small sample of the specimen was cut using a diamond
blade saw. The sample was fixed on two-way sticky tape of 1cm diameter. The sample
was outgassed to remove any air by the use of a rotary pumped coater and thereafter
coated with a gold coating three times. The sample was placed on the platform of the Leo
1450 SEM machine. The chamber of the machine was vented and was then ready for the
SEM analysis.

Figure 32: LEO 1450 SEM Figure 33: Rotary pumped coater

3.6. Chapter summary


This chapter particularized the experimental procedures that were performed in order to
meet the aim and objectives stipulated in chapter 1. The experimental investigations
conducted were selected based on time, funding, availability limitations and the
suitability to the research topic, hence many alternative methods specified in section 2.5.6
had to be omitted. The methods specified in this chapter have been performed according
to the SANS/SABS standards but may have deviated slightly due to the limitation
mentioned in section 4.8.

40
CHAPTER 4: RESULTS AND DISCUSSION
4.1. Introduction
The following chapter will present the results obtained from the experimental procedures
that were used to meet the aims and objectives of this research. The results will be
displayed in summarized graphs and tables and will be followed by a discussion. The
initial intricate data used to obtain the summarized results can be found in appendix B.
The chapter will furthermore elaborate on the results obtained from experimental
procedures to determine the material properties; constituent contents; final mix designs
and the results obtained from the analysis of fresh properties tests, mechanical properties
tests and durability tests.

4.2. Material properties


4.2.1. Fineness modulus by sieve analysis

The fineness modulus of the fine aggregate was determined to be 2.3 from the sieve
analysis. This raw data is presented in section B.1. Figure 34 shows the grading curve for
the fine aggregate. The fine aggregate is relatively well graded from the curve obtained.

GRADING CURVE
100
90
Percentage passing (%)
80
70
60
50
40
30
20
10
0
0,01 0,1 1 10 -10

Sieve size (mm)

Figure 34: Fine aggregate grading curve

41
4.2.2. Coarse aggregate

The stone content was calculated considering the use of a nominal maximum stone size
of 19mm and moderate vibration using the vibrating table. Table 4 and equation 5 was
used to determine the stone content to be 1113 kg/m3.

4.2.3. Water-Binder ratio and water requirement

From the graph and data provided by NPC in figure 54 located in the appendix, a water-
binder ratio of 0.54 was selected to achieve a compression strength of 40MPa. A water
requirement of 210kg/m3 was used according to table 5 for a maximum nominal stone
size of 19mm.

4.3. Mix design


The mix design followed the method specified in section 3.3 and was adjusted
accordingly to provide a workable concrete mix with a 40-70mm slump which is
generally used for most structural elements (Day et al., 2013). The inclusion of
metakaolin in the mix decreased the workability, therefore, to increase the workability
without the use of water reducers/super plasticizers the water-binder ratio was increased.

Table 8: Final Mix design for 1m3

0% MK 5% MK 10% MK 15% MK 20% MK


W-B ratio 0.54 0.54 0.57 0.58 0.61
Water (kg) 210,0 210,0 210,0 210,0 210,0
Cement (kg) 389 369,4 331,6 307,8 275,4
Stone (kg) 1113 1113,4 1113,4 1113,4 1113,4
Sand (kg) 648 648,2 666,1 672,0 687,6
Metakaolin (kg) 0,0 19,4 36,8 54,3 68,9

Table 9: Actual mix design for required volume of 0.09m3

0% MK 5% MK 10% MK 15% MK 20% MK


W-B ratio 0.54 0.54 0.57 0.58 0.61
Water (kg) 19,0 19,0 20,5 20,5 21,5
Cement (kg) 35 33 32 30 28
Stone (kg) 101 101 101 101 101
Sand (kg) 59 58 60 58 57
Metakaolin (kg) 0,0 1,8 4,0 5,0 7,0

42
4.4. Fresh mix properties
The addition of metakaolin significantly reduced the workability of the concrete mix,
therefore the water-binder ratio was adjusted to regulate the slump to be in the 40mm-
70mm range. Figure 35 and 36 show the reduction in slump between the control mix and
15% metakaolin contents for a 0.54 water-binder ratio. The water binder ratio was kept
constant for the 0% and 5% metakaolin additions at 0.54 and was then increased to 0.57,
0.58, 0.61 for the 10%, 15% and 20% inclusions of metakaolin respectively as seen in
figure 37.

Figure 35: Slump for 0% MK Figure 36: Slump for 15%MK

WATER-BINDER RATIO USED


0,62 0,61

0,6
0,58
W/B RATIO

0,58 0,57

0,56
0,54 0,54
0,54

0,52

0,5

0% 5% 10% 15% 20%

Figure 37: Water binder ratio used

43
Figure 38 shows the slump values and water-binder ratios for each mix. The first bar
(blue) shows the slump obtained when a 0.54 water binder was used and the second bar
(red) shows the slump obtained when the adjusted water-binder ratio was used.

FRESH MIX PROPERTIES


80 0,62
70
70
60 0,6
60 55
50
SLUMP (mm)

W/B RATIO
0,58
50 42
40 0,56
30
0,54
20
0,52
10
0 0,5
0% 5% 10% 15% 20%

0,54 W/B Slump 40-70 mm Slump - W/B used W/B ratio used

Figure 38: Fresh mix properties

The 0.54 water-binder ratio decreased the slump values for all additions of metakaolin
and exhibited an extreme decrease in the slump for additions greater than 5%. The
metakaolin utilized majority of the water due to its high surface area stemming from the
fineness of the particles. Without the use of superplasticizer and to prevent wastage of the
mix, additional water was added to provide a suitable slump of 40-70mm. By adding
water, the water-binder ratio was increased and this would in turn result in a decrease in
the mechanical properties of the mix (not considering the effect of the addition of
metakaolin).

The addition of metakaolin resulted in low excess water in the concrete which produced
a ‘stiff’ mix, but after compaction by the vibrating table, a suitable finish was achieved.
It was noted that after placing the concrete in the moulds, vibrating and allowing to rest,
the inclusion of metakaolin resulted in a decrease in the bleeding of the concrete. The
reduction in the bleeding can be credited to the fineness of the metakaolin and the filler
effect which replaced voids and pores in the concrete, preventing the rise of water through
capillaries and the settlement of larger particles.

44
The following temperatures where obtained from the mix immediately after mixing and
before the concrete was filled into the moulds.

TEMPERATURE
25 23
21
20 19
17 17
DEGREES (C)

15

10

0% 5% 10% 15% 20%

Figure 39: Fresh mix temperature

The results indicate that the use of metakaolin decreases the temperature of the mix. This
may be due to the decreased hydration reaction considering that the cement content was
replaced by metakaolin. The metakaolin which is a pozzolanic material does not
contribute to the hydration reaction of cement, therefore there is a reduction in the heat
from the decreased hydration reaction in the mix. In addition, the lower heat produced by
the mix will result in a decrease in shrinkage cracks therefore resulting in further
durability enhancement. The increase in the water-binder ratio may also contribute to the
reduction in the temperature of the concrete after mixing.

The concrete finishing was seen to improve with an increase in metakaolin. The inclusion
of metakaolin produced a lighter coloured mix with a smooth and ‘creamy’ texture. This
made the finishing of the exposed surface of the mould easier and aesthetically pleasing
(pictures available in appendix C). The inclusion of metakaolin also resulted in less air
voids on the surfaces of the cast concrete and the surfaces were smoother than
conventional concrete. The inclusion of metakaolin also reduced the efflorescence of the
concrete; handling the dry samples with high metakaolin produced less of the powder
effect than the samples with lower metakaolin contents.

45
4.5. Mechanical properties
4.5.1. Compression strength

The compressive strength is one of the most important properties of concrete as concrete
is used predominantly for its compressive resistance. If the concrete fails to achieve the
minimum specified 28th day strength with allowance for error, the concrete may not be
acceptable in use.

Figure 40 shows the average results obtained from the compressive strength tests of 3
cubes per mix. The rate of loading was unknown due to the limitations of the machine,
but was kept at a constant rate for all tests.

COMPRESSION STRENGTH VS TIME


0%MK 5%MK 10%MK 15%MK 20%MK

60

50
STRENGTH (MPA)

40

30

20

10

0
0 10 20 30 40 50 60
TIME (DAYS)

Figure 40: Compressive strength over time

The results suggest that all samples gain rapid early strengths (7th day) and gradually
increase in strength for the 28th and 56th day strengths. There is variation in optimal
strengths with respect to time which could be a result of the availability of the calcium
hydroxide for the pozzolanic reaction and the dilution effect.

46
7th day results show an optimum metakaolin content of 10% followed by the 15%, 0%,
5% and 20%. The reason for the low early strength in the 20% metakaolin inclusion could
be a result of insufficient calcium hydroxide production from the hydration reaction to
initiate the pozzolanic reaction. The increased water-binder ratio would also decrease the
strength of the 10%, 15% and 20%; in spite of this the 10% and 15% show significant
strength improvement over the lower water-binder ratios and the control mix.

28th day results show an optimum metakaolin content of 5% with 10% tailing very closely
followed by 15%, 20% and then 0%. The 28 day strengths of all metakaolin inclusions
produce higher strengths than the control mix despite the higher water binder ratio. It is
highly possible that the 10% can be seen as the optimum if the water binder ratios were
the same and this would be similar for the 15% and 20%.

56th day tests were done as an extra test and was not cured according to the standard
specifications, instead they were cured under moist conditions with a damp fabric 7 days
prior to testing. The results suggest that 10% metakaolin content is the optimum followed
by 5%, 0%, 15% and 20%. Once again the increased water-binder ratio has a significant
effect in reducing the compressive strengths for 10%. 15% and 20%.

COMPRESSION STRENGTHS
COMPRESSIVE STRENGTH (MPA)

60,00

50,00

40,00

30,00

20,00

10,00

0,00
0%MK 5%MK 10%MK 15%MK 20%MK
7 day 22,76 22,49 27,76 25,00 19,69
28 day 33,49 42,43 41,21 36,79 36,33
56 day 43,42 46,63 49,80 41,72 41,22

Figure 41: Compressive strengths vs percentage metakaolin

47
Figure 42 is a comparison between the actual results obtained from the designed mix and
the estimated minimum and estimated average results provided by NPC for the respective
water-binder ratios. The conceptual design aimed to used 0.54 water-binder ratio to
achieve a target strength of 40MPa, however the actual strength obtained was 33.5 MPa
which could have occurred due to factors such as the material influences, rate of loading
of machines and errors mentioned in section 4.8. The aforementioned influences were
assumed to have remained constant for all mix designs so that comparisons could be
drawn. Considering that the design mix was lower than the estimated minimum strength,
it can be assumed that the design mixes for all water-binder ratios with a 0% metakaolin
inclusion would be lower than the estimated minimum; and similarly the design mixes
for the metakaolin inclusions should be lower than the estimated minimum strengths.
Despite the previous statement, the inclusion of metakaolin has significantly increased
the actual strength of the concrete greater than the estimated minimum.

28 DAY COMPRESSIVE STRENGTHS


COMPRESSIVE STRENGTH (MPa)

COMPARISON
50,00

40,00

30,00

20,00

10,00

0,00
0,57 0,59 0,61
0,54 (0MK) 0,54 (5MK)
(10MK) (15MK) (20MK)
Actual Strength 33,49 42,43 41,21 36,79 36,33
Estimated Minimum 40,2 40,2 37,3 35,37 33,53

Figure 42: 28th day compressive strength comparison

The increase in compressive strength with the inclusion of metakaolin can be credited to
the filler effect and high pozzolanic reactions. The pozzolanic reactions between the
calcium hydroxide and the silica and alumina components of metakaolin resulted in the
formation of calcium silicate hydrates which significantly increased the strength of the
concrete due to the cementing properties. The reduction in strength in the 20% can be
seen as a result of the dilution effect; whereby the high content of metakaolin had used
up its calcium hydroxide resources and were unable to react further.

48
4.5.2. Flexural strength

The flexural strengths were tested with beams as specified in section 3.2.6. All beam
samples for the flexural tests were cured under moist conditions with a damp fabric due
to the limitations as specified in section 4.8.

Figure 43 shows the average results obtained from the flexural strength tests of 3 beams
per mix. The rate of loading for the tests were unknown due to the limitations of the
machine, but it was kept constant for all tests to ensure relative comparisons.

FLEXURAL STRENGTH VS TIME


0%MK 5%MK 10%MK 15%MK 20%MK

5
STRENGTH (MPA)

0
0 10 20 30 40 50 60
TIME (DAYS)

Figure 43: Flexural strength over time

The results suggest that all samples gain rapid early strengths (7th day) and gradually
increase in strength for the 28th and 56th day strengths. There is variation in optimal
strengths with respect to time which could be a result of the availability of the calcium
hydroxide for the pozzolanic reaction and the dilution effect. The flexural results portray
similar correlation to the compression strengths seen in section 4.5.1 with an exception
for the 56-day results which varied from the trends due to possible errors.

49
7th day flexural results suggest an optimal metakaolin inclusion of 10% followed by 15%,
5%, 0% and 20%. Similarly, to the compression results, the 20% inclusion of metakaolin
showed low early strength in comparison to the other percentages due to the limited
calcium hydroxide production which is essential for the pozzolanic reaction of
metakaolin. In addition, the increased water-binder ratios result in a decrease in flexural
strength of the specimens.

28th day results suggest an optimal metakaolin content of 5% closely tailed by the 10%
and followed by 15%, 20% and 0%. The 28 day strengths of all metakaolin inclusions
produce higher strengths than the control mix despite the increased water-binder ratio. It
is highly possible that the 10% can be seen as the optimum if the water-binder ratios were
the same and this would be similar for the 15% and 20%.

56th day results suggest that 5% metakaolin content is the optimum followed by 20%,
10%, 15% and 0%. Once again the increased water-binder ratio has a significant effect in
reducing the compressive strengths for 10%. 15% and 20%, however the 20% shows an
extremely high flexural strength. There could be a possibility of error for the 10% and
15% or the 20% flexural results.

FLEXURAL STRENGTHS
FLEXURAL STRENGTH (MPA)

5,5

4,5

3,5

3
0%MK 5%MK 10%MK 15%MK 20%MK
7 day 3,6 3,74 3,83 3,81 3,37
28 day 4,4 4,76 4,66 4,56 4,56
56 day 4,61 5,01 4,74 4,66 4,935

Figure 44: Flexural strengths vs percentage metakaolin

50
4.5.3. Further Evaluation

Figure 45 shows the percentage increase in compressive and flexural strengths at 28 days
in comparison to the control mix. The compressive and flexural strengths show a similar
trend and will therefore be compared together. The compression test results show a
significant increase of 26.7% for 5% metakaolin inclusion and the percentage decreases
with higher metakaolin contents due to the increase in the water-binder ratio. The flexural
test results show the highest increase of 8.18% for 5 % metakaolin inclusion and the
percentage decreases with increasing metakaolin content due to the increase in the water-
binder ratio.

The decrease in the ‘percentage increase of strength’ over the increasing metakaolin
replacement percentage is primarily a result of the increased water-binder ratio that was
used. If all water-binder ratios were kept constant it is possible to see a different trend
whereby the 10%,15% and 20% metakaolin contents would show a significant increase
in strength and may perform better than the 5% metakaolin addition.

28 DAY - PERCENTAGE INCREASE


30,00
26,67

25,00 23,05
PERCENTAGE %

20,00

15,00
9,84
10,00 8,18 8,47
5,91
3,64 3,64
5,00

0,00
5% 10% 15% 20%
Flexure 8,18 5,91 3,64 3,64
Compression 26,67 23,05 9,84 8,47

Figure 45: 28 day percentage increase in strengths

51
4.6. Durability
4.6.1. Mass, Density and absorption

Figure 46 shows the average density for samples tested at 56 days in air dried conditions
and the water-binder ratio for each mix. The inclusion of metakaolin can be seen to
increase the density of concrete when comparing the 0% and 5% metakaolin additions
with the same water-binder ratio. Due to its fine particle size of 2 micro meters,
metakaolin is able to act as a filler and reduce voids and pores in the concrete resulting in
a closely packed and denser mix. The increase in the water-binder ratio resulted in a
decrease of the samples density and therefore an accurate comparison of the densities
could not be performed.

AVERAGE DENSITY
2410 2400 0,62
2400
2390 2384 0,6
2380 2373

W/B RATIO
MASS (g)

2367 0,58
2370
2360 0,56
2350 2343
2340 0,54
2330 0,52
2320
2310 0,5
0%MK 5%MK 10%MK 15%MK 20%MK

Density W/B Ratio

Figure 46: Average dry density

The samples were also weighed at the fully saturated state (straight from the water bath)
and after being allowed to air dry for 7 days (unsaturated). The results are shown in figure
47. The trends specified for the density evaluation in figure 46 also corresponds with the
saturated and unsaturated mass of the samples displayed in figure 47. The results further
indicate that the inclusion of metakaolin reduced the absorption ability of the concrete.
This can be seen by the decreasing percentage absorption between 0% and 5%, however
due to the increase in the water-binder ratio, the 10%, 15% and 20% percentage
absorption cannot be accurately compared. Despite the fact that there was a slight increase
in the water-binder ratio for 15% inclusion of metakaolin, it is able to show a reduction
in percentage of water absorption compared to the 10% metakaolin content.

52
MASS AND WATER ABSORPTION
Saturated mass Unsaturated mass Percentage absorption
8150 0,58

Percentage absorption (%)


8100
0,56
Mass (g)

8050
8000 0,54
7950 0,52
7900
7850 0,50
7800 0,48
7750
0,46
7700
7650 0,44
0%MK 5%MK 10%MK 15%MK 20%MK

Figure 47: Mass and water absorption

From the results obtained from the water absorption, an indication of the porosity could
be determined. The water absorbed by the concrete gives an indication of the pores within
the concrete and therefore the pore volume percentage would correspond to the
percentage of water absorbed in figure 47.

4.6.2. Water sorptivity

Figure 48 presents the water sorptivity results of the specimen from the method explained
in section 3.5.3 and the raw data from the experiment which can be located in appendix
B. The method was conducted without the use of a desiccator, therefore, the saturated
mass was obtained at atmospheric pressure.

The results in figure 48 indicate that there is a decrease in the water absorption when
metakaolin is included in the concrete mix. Despite the increase in the water-binder ratio,
the 10% proved to be the optimal in resisting water absorption due to capillary rise, thus
indicating fewer capillaries in the microstructure. The fewer capillaries due to the filler
effect of metakaolin can indicate that there are reduced pores and therefore an overall
increased durability of the concrete. The water sorptivity rises with 15% and 20%
metakaolin additions which could be a result of the increased water binder ratio or due to
an increase in capillaries indicating that 10% is the optimum.

53
WATER SORPTIVITY
6,00 0,62

AVERAGE SOPTIVITY (mm/√hr)


5,00 0,6

4,00 0,58

W/B RATIO
3,00 0,56

2,00 0,54

1,00 0,52

0,00 0,5
0%MK 5%MK 10%MK 15%MK 20%MK
WS 4,86 4,45 2,26 3,57 3,79
W/B 0,54 0,54 0,57 0,58 0,61

Figure 48: Water sorptivity

4.6.3. Air Permeability

From the method specified in section 3.5.4, the following results were obtained.
Experimental tests that exceeded 1000s were stopped and classified as excellent.

Table 10: Air permeability results

Time (s) AER (s/ml) Category


0% MK 217 53.60 Fair
5% MK 857 211.68 Good
10% MK > 1000 > 250 Excellent
15% MK > 1000 > 250 Excellent
20% MK > 1000 > 250 Excellent

The air permeability performed by the porosiscope test produced the following results.
The results were unable to provide a distinguishable difference in the samples after the
1000s time allocation. However, the trend can be seen that an increase in metakaolin
content significantly reduces the air permeability of the concrete. This is a result of the
decreased pores and increased durability properties of the concrete by adding metakaolin
and this can be supported by the results obtained from past experiments.

54
4.6.4. Water permeability

From the method specified in section 3.5.4, the following results were obtained.
Experimental tests that exceeded 1000s were stopped and classified as excellent.

Table 11: Water permeability results

Time (s) WAR (103 s/ml) Category


0% MK 227 22.7 Fair
5% MK 493 49.3 Good
10% MK 560 56.0 Good
15% MK 589 58.9 Good
20% MK 619 61.90 Good

The water permeability performed by the porosiscope test produced the following results.
The trend can be seen that an increase in metakaolin content significantly reduces the
water permeability of the concrete. This is a result of the decreased pores and increased
durability properties of the concrete by adding metakaolin and this can be supported by
the results obtained from past experiments.

4.7. Scanning Electron Microscope

Pores

Void

Cement
particle

Figure 49: 0% Metakaolin content

55
Pore

Micro-
cracks

Void

Figure 50: 5% Metakaolin content

Void

Figure 51: 10% Metakaolin content

56
Figure 52: 15% Metakaolin content

Figure 53: 20% Metakaolin content

57
Figures 49 to 53 provide the SEM images for the 0%, 5%, 10%, 15% and 20% metakaolin
contents respectively. The control mix (figure 49) displays concrete with a large number
of voids and pores. On the contrary, the addition of metakaolin (figures 50 to 53) can be
perceived to reduce the voids and pores by producing a cohesive matrix of calcium silicate
hydrate gels which is noted to increase with the increasing metakaolin additions. The
influence of the increase in these gels and the reduction of calcium hydroxide was
explained in section 2.5.1 to improve the mechanical and durability properties of
concrete.

4.8. Limitations and Errors


 Due to the large number of students requiring the use of the curing rooms. The
samples were curing in the curing room at a controlled temperature for the first
6/7 days. Thereafter, the cubes were placed in a water bath and the beams were
covered in damp cloths and kept moist.
 Resulting from poor workability and low slump of the concrete with the inclusion
of metakaolin, the water-binder had to be changed by adding water to adjust the
concrete to a desired slump.
 Material, time, equipment and funding limitations reduced the number of samples
produced and thus limiting the accuracy of results obtained and the various tests
that could be done for this research. This also prevented the use of additional
admixtures such as superplasticizers.
 The rate of loading for the compression and flexural testing equipment were
unknown, consequently affecting the results as the strength of the concrete is
influenced by the rate of loading. However, all rates of loading were kept constant
for all strength tests.
 The time restrictions on this research also prevented the chance to redo and correct
errors/flaws in the design. The time constraints also influenced the ability to
perform various durability tests which require a considerable amount of time to
perform.
 The research planned to assess the influence of metakaolin in conventional
concrete without the use of superplasticizers. The higher percentage inclusions of
metakaolin resulted in a mix with low workability and therefore resulted in the
water-binder ratio being changed to achieve suitable workability.

58
 Durability tests for the air permeability was stopped after the limit of 1000s which
classified the sample as excellent in the resistance to air permeability. This was
due to the time allocation of Naidu Consultants to the students and the actual time
of the test could not be estimated.
 Outcomes resulting from the SEM imaging were interpreted to the best of the
student’s ability due to lack of expertise and knowledge in that field.

Errors

 Inaccurate results could be due to the curing issues mentioned in the limitations.
 Due to the varying water-binder ratios for the mixes, it was difficult to obtain an
accurate comparison of the influence of increasing the metakaolin percentage to
find an optimum.
 Inaccurate results could be due to errors in the mix design, calculations, or the
actual measuring, mixing and vibration of the concrete due to human error
 Inaccurate results can be due to poorly calibrated lab equipment. The rate of
loading for the compression and flexural tests were unknown and this could have
been one of the reasons the target strength was not met.
 The moulds were in a poor condition and not perfectly square. This resulted in
poorly shaped samples which had varying cross sectional areas which impacts the
results obtained from the tests. The poorly shaped samples may also cause
eccentric loading when subjected to the mechanical tests, thus resulting in
inaccurate results.

4.9. Chapter Summary


This chapter presented the results obtained from the experimental investigations
described in chapter 3 which was required to fulfill the aims and objectives from chapter
1. The raw data from the experiments were input into an excel spreadsheet, the relevant
calculations were performed, tables were developed (which can be seen in appendix B)
and the summarized results were used to generate suitable graphs. The use of the graphs
makes it simpler to communicate and compare the results obtained. The graphs are
explained and discussed, critically analyzing the results that were produced. The
limitations and errors were mentioned and the results that were discussed will be
concluded in chapter 5.

59
CHAPTER 5: CONCLUSION AND RECOMMENDATIONS
5.1. Conclusion
The overall experimental investigation has noted that the addition of metakaolin
significantly enhances the mechanical and durability properties of concrete. Despite the
increase in the water-binder ratio for the 10%, 15% and 20% additions of metakaolin,
these concrete mixes exhibited a higher standard (in terms of majority of the properties
analyzed) than the control mix at a lower water-binder ratio. This could also indicate that
higher water binder ratios with the inclusion of metakaolin can be used to achieve the
strengths and properties produced by conventional concrete with lower water-binder
ratios which may be a considerably cheaper alternative. Metakaolin is relatively
expensive when compared to ordinary cement, however, the life cycle analysis of the
economic impacts should be considered.

The area where the use of metakaolin fails to improve the properties of conventional
concrete would be concerning the influence on workability of the fresh concrete. This
will be concluded further in section 5.1.1.

5.1.1. Fresh mix properties

The results indicate that an increase in metakaolin decreases the workability of the mix
therefore a lower slump was found. The reduction in workability may be a result of the
increased surface area due to the finer particle size of metakaolin; or could be a result of
the water absorption properties of metakaolin resulting in less water for the concrete mix.
A substantial amount of water was required in order to increase the slump and workability
to a suitable value.

There is a decrease in temperature of the concrete mix when the metakaolin content is
increased (despite the increased water-binder ratio). This may be possible due to the
reduced hydration reaction as there is a lower percentage of cement in the mix. The
decrease in temperature will also result in a reduction in shrinkage cracks, thus enhancing
the durability properties of the mix.

60
5.1.2. Mechanical properties

The compression and flexural properties displayed a similar trend with the results stating
that an increase in metakaolin contents substantially increased the compression and
flexural strengths of the concrete. All metakaolin contents exhibited higher strengths than
the control mix for the 28 day tests despite the increased water-binder content which
should have significantly reduced the concrete strength. The use of metakaolin has been
proven to be highly advantageous in increasing the mechanical properties of conventional
concrete.

5.1.3. Durability

The durability testing of the samples were quite difficult perform due to the limited
equipment available and the expertise required for the tests. The air and water
permeability tests performed by Naidu consulting provided results that indicated that the
increase in metakaolin content yielded a substantial decrease in the air and water
permeability of the samples. This can be attributed to the filler effect from the fineness of
the metakaolin particles and the additional calcium-silicate hydrate gels which reduced
the number and sizes of the pores resulting in a less permeable concrete.

The average densities were determined by weighing the samples and recording the
dimensions of the sample to obtain the volume. The results were able to conclude that an
increase in metakaolin made the concrete denser. In addition, the water absorption of the
concrete sample was determined by weighing the sample straight out of the water bath
(fully saturated) and weighing the sample after having it air dried for 7 days (unsaturated).
The difference between the saturated and unsaturated mass was able to provide a relative
mass of water absorbed. The results showed that the increase in the metakaolin content
resulted in a decrease in water absorption; and an increase in the water-binder ratio
resulted in an increase in the water absorption. The increase in densities and reduction in
water absorption for the increasing metakaolin content could be a result of the filler effect
caused by the fineness of the metakaolin particles which also reduced pores and voids
creating a closely packed denser concrete in addition to the additional calcium silicate
hydrates being produced.

61
The water sorptivity tests indicate that an increase in the metakaolin content decreases
the water absorption of the concrete from capillary rise, thus indicating a reduction in
capillaries, pores and voids which suggests an enhancement in durability properties.
Although this test was not performed accurately due to the lack of a desiccator and errors
mentioned in section 4.8, the results provided an adequate correlation to the outcomes
obtained from the alternative experimental investigations performed which indicated that
the inclusion of metakaolin significantly reduces the water absorption, thus enhancing the
durability properties of the concrete by its resistance to the transportation of deleterious
substances in the concrete.

The SEM imaging results were the best images that could be obtained at the time, as the
alternative advanced imaging equipment had been overbooked and time constraints were
taken into consideration. The interpretation and conclusions of the images were limited
due to the lack of experience and knowledge in this field but has been included in this
report for future reference. Nevertheless, the images were able to indicate that increase in
metakaolin increased the production of calcium silicate hydrate gels which occupied
pores, voids and capillaries indicating an enhancement in mechanical and durability
properties.

In correlation to the mechanical and durability tests, the following relationships were
derived. Mechanical and durability property enhancement was achieved by:

 A reduction in pores and voids ensuing from the filler effect of the fine
metakaolin particles (thus attaining a dense closely packed microstructure) which
reduced the pore content for strength and reduced the transportation properties of
deleterious substances.
 A reduction in dormant calcium hydroxide which offered no benefits to the
mechanical properties in conjunction with an increase in calcium silicate hydrates
which formed cementitious compounds occupied pores and voids contributed to
the strength enhancement and reducing the transportation properties of
deleterious substances.
 The use of metakaolin exhibited a reduction in micro cracks which could stem
from the decrease in the hydration temperature hence decreased drying shrinkage.
62
5.1.4. Environmental, economic and social impacts

Environmental

The manufacture of metakaolin is only responsible for the emission of CO2 during
extraction (surface mined, therefore low emission), transportation but predominantly
during calcination which takes place at 700-800 degrees celsius. However, this is
significantly lower than the CO2 emissions for Portland cement which comprise of
extraction, transportation, calcination at 1500 degrees celsius (large emission from coal
powered energy) and an additional emission from the byproduct of calcining limestone.

Economic

The cost of metakaolin in South Africa according to Serina Trading Company is R9 per
kg which is approximately to R518 per 50kg bag after VAT (the invoice can be seen in
appendix A.3). This is quite expensive compared to the NPC cement that was used which
is approximately R80 per 50kg bag, however it may be possible to obtain discounts for
metakaolin bought in bulk. Despite the large cost implications with metakaolin, it is
possible that it can be the cheaper option when considering the total life of the structure;
the enhanced durability compared to conventional concrete which will require more
maintenance; and smaller section sizes due to the improved compression strength. The
time limit given to this dissertation topic did not allow for a detailed economic analysis
for the inclusion of metakaolin and the comparison to conventional concrete in the short
and long term. The use of metakaolin may prove to be more beneficial in High and Ultra
High Performance concrete compared to conventional concrete. High performance
concretes are used for highly stressed structures that are exposed to harsh environments
where durability and strength cannot be compromised.

Social

The kaolin industry is relatively unoccupied in South Africa and there is great potential
in this market as seen in section 2.4.7. The exploration of this market can result in an
overall boost in the South African economy due to the increase in jobs that will be created,
the increase in trade and exportation and an improvement in the infrastructure and design
of structures in South Africa.
63
5.2. Recommendations
It is evident that the inclusion of metakaolin significantly increases the mechanical and
durability properties of concrete. The economic analysis suggests that cost of metakaolin
per kg is significantly higher than cement. Although the costs of including metakaolin
may be cheaper when considering the effect of durability and the life cycle of the
structure, most construction industries fail to see this due to the expensive initial costs.
Recommended metakaolin contents from past research indicate no more than 30%
metakaolin to be used due to adverse effects, thus still requiring the use of a substantial
amount of cement which still has a significant impact on the environment.

From the aforementioned evaluation, a recommendation to use another supplementary


material in conjunction with metakaolin may prove to be a better alternative. From past
research most SCM’s such as fly-ash and waste paper sludge tend to reduce the
compressive strength of concrete. However, with the inclusion of metakaolin in
conjunction with the other SCM’s the following can be achieved:

 Low strengths, slow setting times and poor durability properties of SCM’s can be
enhanced by the use of metakaolin to that similar if not better than usual concrete.
 Balancing the low cost of SCM’s with the high cost of metakaolin may yield
reasonable pricing, thus promoting sustainable concrete.
 The high workability of SCM’s with the low workability of metakaolin can omit
of using superplasticizers (as seen in figure 15 of section 2.4.5.2).

5.3. Future scope/research


 The use of metakaolin in geopolymer concrete, high or ultra-high performance
concrete.
 Determine the optimal metakaolin content using a constant water-binder ratio for
all metakaolin contents. This would require the use of super plasticizers.
 Further research into the durability of concrete with metakaolin.
 Assess the influence of curing methods on concrete with metakaolin.
 Assess the influence of metakaolin in conjunction with other supplementary
cementitious materials. As explained in the recommendations.

64
REFERENCES
Abdul Razak H, Chai HK and Wong HS. (2004) Near surface characteristics of concrete
containing supplementary cementing materials. Cement and Concrete
Composites 26: 883-889.
Abdul Razak H and Wong HS. (2005) Strength estimation model for high-strength
concrete incorporating metakaolin and silica fume. Cement and Concrete
Research 35: 688-695.
Aiswarya S, Prince Arulraj G and Dilip C. (2013) A review on use of metakaolin in
concrete. Engineering Science and Technology 3: 592-597.
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69
APPENDICIES
APPENDIX A: Data and pre mix calculations
A.1. Water-Binder ratio vs Strength

W/C RATIOS vs CEMENT TYPE - NPC


CHARACTERISTIC/MINIMUM STRENGTH
60

55

50

45
28 - Day Strength [MPa]

40

35

30

25

20

15

10
0,4 0,5 0,6 0,7 0,8 0,9 1
W/C Ratio

NPC PRO - CEMIIIA-S 32.5N

NPC PLUS - CEMIIB-S 42.5N

NPC PREMIUM - CEMIIA-S 42.5N

Figure 54 : Water-Cement ratios for desired strengths

70
A.2. Sample Calculations

 Mix design volume

Table 12: Mix design volume required

VOLUME REQUIRED
Moulds Volume Number Totals Units
Cubes 0,003375 10 0,03375 m3
Beams 0,005 9 0,045 m3
Cylinders 0,005301 0 0 m3
Required Volume 0,079 m3
15% added for wastage 0,091 m3 per mix design

water/binder ratio 0,54


required water per m3 210

 Conceptual Mix design

Table 13: Conceptual mix design per cubic meter

CONCEPTUAL DESIGN PER CUBIC METER


Mass (kg) 0% MK 5% MK 10% MK 15% MK 20% MK
Water 210,0 210,0 210,0 210,0 210,0
Cement 388,9 369,4 331,6 307,8 275,4
Stone 1113,4 1113,4 1113,4 1113,4 1113,4
Sand 647,6 644,4 659,1 661,6 674,5
Metakaolin 0,0 19,4 36,8 54,3 68,9

Table 14:Conceptual design per mix

CONCEPTUAL DESIGN PER MIX


Mass (kg) 0% MK 5% MK 10% MK 15% MK 20% MK
Water 19,0 19,0 19,0 19,0 19,0
Cement 35 33 30 28 25
Stone 101 101 101 101 101
Sand 59 58 60 60 61
Metakaolin 0,0 1,8 3,3 4,9 6,2

Table 15: Actual design per mix

ACTUAL DESIGN PER MIX


Mass (kg) 0% MK 5% MK 10% MK 15% MK 20% MK
Water 19,0 19,0 20,5 20,5 21,5
Cement 35 33 32 30 28
Stone 101 101 101 101 101
Sand 59 58 60 58 57
Metakaolin 0,0 1,8 4,0 5,0 7,0

71
CONCRETE MIX DESIGN
CLIENT: STUDENT No 213506133 PROJECT:Dissertation
REQUIREMENTS: STRENGTH: 40 MPa SLUMP: 40-70 mm W/C: 0,54

MATERIAL TYPE AND SOURCE SIZE RD: LBD CBD FM K VALUES HAND MOD HEAVY
[mm] [kg/m^3] [kg/m^3} STONE COMP VIBR VIBR
CEMENT NPC PRO - CEMIIB-S 42.5N 3,1 9,5 0,75 0,8 1
METAKAOLIN HIGH REACTIVITY - K40 2,6 13,2 0,84 0,9 1,05
STONE 1 TILLITE 19 2,65 1360 1446 19,0 0,94 1 1,05
STONE 2 26,5 1 1,06 1,1
SAND 1 UMGENI RIVER SAND 2,65 1320 1400 2,30 FOR CBD [kg/m^3} 1446
SAND 2 STONE 19
PERCENTAGE METAKAOLIN Dosage: 0 % mass SELECTED K 1
1 m^3 (1000 l) NOTE: kg/RD = litres STONE REQD [kg] 1113,42

STONE REQUIRED [from chart using stone size and FM of sand] 1113,42 kg

MIX 1 MIX 2 MIX 3 MIX 4


MATERIAL kg litre kg litre kg litre kg litre
WATER 240 240 230 230 220 220 210 210
CEMENT 444 143 426 137 407 131 389 125
METAKAOLIN 0 0 0 0 0 0 0 0
STONE 1 1113 420 1113 420 1113 420 1113 420
STONE 2 0 0 0 0 0 0 0 0
SAND 1 521 196 563 212 605 228 648 244
SAND 2 0 0 0 0 0 0 0 0
ADMIXTURE 0 ml 0 0 0
TOTAL 2319 1000 2332 1000 2346 1000 2360 1000
FACTOR mix size/1000 x (w ater mix 1)/(w ater mix X)
0,0792 0,0792 0,0827 0,0864 0,0906

LAB MIX
MIX 1 MIX 2 MIX 3 MIX 4
MATERIAL kg Litre Add kg kg Litre Add kg kg Litre Add kg kg Litre
WATER 19,0 19,0 0,0 19,0 19,0 0,0 19,0 19,0 0,0 19,0 19,0
CEMENT 35,2 11,4 0,0 35,2 11,4 0,0 35,2 11,4 0,0 35,2 11,4
METAKAOLIN 0,0 0,0 0,0 0,0
STONE 1 88,2 33,3 3,8 92,1 34,7 4,2 96,3 36,3 4,6 100,8 38,1
STONE 2
SAND 1 41,3 15,6 5,3 46,6 17,6 5,8 52,3 19,7 6,3 58,7 22,1
SAND 2
ADMIXTURE 0,0 0,0 0,0 0,0
Total 183,7 79,2 192,9 82,7 202,8 86,4 213,7 90,56

SLUMP mm mm mm 70 mm

Comments:
Mix done by: Date:
Cubes marked:

Figure 55: 0% metakaolin mix design

72
CONCRETE MIX DESIGN
CLIENT: STUDENT No 213506133 PROJECT:Dissertation
REQUIREMENTS: STRENGTH: 40 MPa SLUMP: 40-70 mm W/C: 0,54

MATERIAL TYPE AND SOURCE SIZE RD: LBD CBD FM K VALUES HAND MOD HEAVY
[mm] [kg/m^3] [kg/m^3} STONE COMP VIBR VIBR
CEMENT NPC PRO - CEMIIB-S 42.5N 3,1 9,5 0,75 0,8 1
METAKAOLIN HIGH REACTIVITY - K40 2,6 13,2 0,84 0,9 1,05
STONE 1 TILLITE 19 2,65 1360 1446 19,0 0,94 1 1,05
STONE 2 26,5 1 1,06 1,1
SAND 1 UMGENI RIVER SAND 2,65 1320 1400 2,30 FOR CBD [kg/m^3} 1446
SAND 2 STONE 19
PERCENTAGE METAKAOLIN Dosage: 5 % mass SELECTED K 1
1 m^3 (1000 l) NOTE: kg/RD = litres STONE REQD [kg] 1113,42

STONE REQUIRED [from chart using stone size and FM of sand] 1113,42 kg

MIX 1 MIX 2 MIX 3 MIX 4


MATERIAL kg litre kg litre kg litre kg litre
WATER 240 240 230 230 220 220 210 210
CEMENT 422 136 405 131 387 125 369 119
METAKAOLIN 22 9 21 8 20 8 19 7
STONE 1 1113 420 1113 420 1113 420 1113 420
STONE 2 0 0 0 0 0 0 0 0
SAND 1 517 195 559 211 602 227 644 243
SAND 2 0 0 0 0 0 0 0 0
ADMIXTURE 0 ml 0 0 0
TOTAL 2315 1000 2329 1000 2343 1000 2357 1000
FACTOR mix size/1000 x (w ater mix 1)/(w ater mix X)
0,0792 0,0792 0,0827 0,0864 0,0906

LAB MIX
MIX 1 MIX 2 MIX 3 MIX 4
MATERIAL kg Litre Add kg kg Litre Add kg kg Litre Add kg kg Litre
WATER 19,0 19,0 0,0 19,0 19,0 0,0 19,0 19,0 0,0 19,0 19,0
CEMENT 33,5 10,8 0,0 33,5 10,8 0,0 33,5 10,8 0,0 33,5 10,8
METAKAOLIN 1,8 1,8 1,8 1,8
STONE 1 88,2 33,3 3,8 92,1 34,7 4,2 96,3 36,3 4,6 100,8 38,1
STONE 2
SAND 1 41,0 15,5 5,3 46,3 17,5 5,8 52,0 19,6 6,3 58,4 22,0
SAND 2
ADMIXTURE 0,0 0,0 0,0 0,0
Total 183,4 78,6 192,6 82,0 202,5 85,8 213,4 89,89

SLUMP mm mm mm 60 mm

Comments:
Mix done by: Date:
Cubes marked:

Figure 56: 5% metakaolin mix design

73
CONCRETE MIX DESIGN
CLIENT: STUDENT No 213506133 PROJECT:Dissertation
REQUIREMENTS: STRENGTH: 40 MPa SLUMP: 40-70 mm W/C: 0,57

MATERIAL TYPE AND SOURCE SIZE RD: LBD CBD FM K VALUES HAND MOD HEAVY
[mm] [kg/m^3] [kg/m^3} STONE COMP VIBR VIBR
CEMENT NPC PRO - CEMIIB-S 42.5N 3,1 9,5 0,75 0,8 1
METAKAOLIN HIGH REACTIVITY - K40 2,6 13,2 0,84 0,9 1,05
STONE 1 TILLITE 19 2,65 1360 1446 19,0 0,94 1 1,05
STONE 2 26,5 1 1,06 1,1
SAND 1 UMGENI RIVER SAND 2,65 1320 1400 2,30 FOR CBD [kg/m^3} 1446
SAND 2 STONE 19
PERCENTAGE METAKAOLIN Dosage: 10 % mass SELECTED K 1
1 m^3 (1000 l) NOTE: kg/RD = litres STONE REQD [kg] 1113,42

STONE REQUIRED [from chart using stone size and FM of sand] 1113,42 kg

MIX 1 MIX 2 MIX 3 MIX 4


MATERIAL kg litre kg litre kg litre kg litre
WATER 240 240 230 230 220 220 210 210
CEMENT 379 122 363 117 347 112 332 107
METAKAOLIN 42 16 40 16 39 15 37 14
STONE 1 1113 420 1113 420 1113 420 1113 420
STONE 2 0 0 0 0 0 0 0 0
SAND 1 534 201 576 217 617 233 659 249
SAND 2 0 0 0 0 0 0 0 0
ADMIXTURE 0 ml 0 0 0
TOTAL 2308 1000 2322 1000 2337 1000 2351 1000
FACTOR mix size/1000 x (w ater mix 1)/(w ater mix X)
0,0792 0,0792 0,0827 0,0864 0,0906

LAB MIX
MIX 1 MIX 2 MIX 3 MIX 4
MATERIAL kg Litre Add kg kg Litre Add kg kg Litre Add kg kg Litre
WATER 19,0 19,0 0,0 19,0 19,0 0,0 19,0 19,0 0,0 19,0 19,0
CEMENT 30,0 9,7 0,0 30,0 9,7 0,0 30,0 9,7 0,0 30,0 9,7
METAKAOLIN 3,3 3,3 3,3 3,3
STONE 1 88,2 33,3 3,8 92,1 34,7 4,2 96,3 36,3 4,6 100,8 38,1
STONE 2
SAND 1 42,3 16,0 5,3 47,6 18,0 5,8 53,4 20,1 6,3 59,7 22,5
SAND 2
ADMIXTURE 0,0 0,0 0,0 0,0
Total 182,9 78,0 192,0 81,4 202,0 85,2 212,9 89,28

SLUMP mm mm mm 55 mm

Comments:
Mix done by: Date:
Cubes marked:

Figure 57: 10% metakaolin mix design

74
CONCRETE MIX DESIGN
CLIENT: STUDENT No 213506133 PROJECT:Dissertation
REQUIREMENTS: STRENGTH: 40 MPa SLUMP: 40-70 mm W/C: 0,58

MATERIAL TYPE AND SOURCE SIZE RD: LBD CBD FM K VALUES HAND MOD HEAVY
[mm] [kg/m^3] [kg/m^3} STONE COMP VIBR VIBR
CEMENT NPC PRO - CEMIIB-S 42.5N 3,1 9,5 0,75 0,8 1
METAKAOLIN HIGH REACTIVITY - K40 2,6 13,2 0,84 0,9 1,05
STONE 1 TILLITE 19 2,65 1360 1446 19,0 0,94 1 1,05
STONE 2 26,5 1 1,06 1,1
SAND 1 UMGENI RIVER SAND 2,65 1320 1400 2,30 FOR CBD [kg/m^3} 1446
SAND 2 STONE 19
PERCENTAGE METAKAOLIN Dosage: 15 % mass SELECTED K 1
1 m^3 (1000 l) NOTE: kg/RD = litres STONE REQD [kg] 1113,42

STONE REQUIRED [from chart using stone size and FM of sand] 1113,42 kg

MIX 1 MIX 2 MIX 3 MIX 4


MATERIAL kg litre kg litre kg litre kg litre
WATER 240 240 230 230 220 220 210 210
CEMENT 352 113 337 109 322 104 308 99
METAKAOLIN 62 24 59 23 57 22 54 21
STONE 1 1113 420 1113 420 1113 420 1113 420
STONE 2 0 0 0 0 0 0 0 0
SAND 1 537 203 578 218 620 234 662 250
SAND 2 0 0 0 0 0 0 0 0
ADMIXTURE 0 ml 0 0 0
TOTAL 2304 1000 2318 1000 2333 1000 2347 1000
FACTOR mix size/1000 x (w ater mix 1)/(w ater mix X)
0,0792 0,0792 0,0827 0,0864 0,0906

LAB MIX
MIX 1 MIX 2 MIX 3 MIX 4
MATERIAL kg Litre Add kg kg Litre Add kg kg Litre Add kg kg Litre
WATER 19,0 19,0 0,0 19,0 19,0 0,0 19,0 19,0 0,0 19,0 19,0
CEMENT 27,9 9,0 0,0 27,9 9,0 0,0 27,9 9,0 0,0 28 9,0
METAKAOLIN 4,9 4,9 4,9 5
STONE 1 88,2 33,3 3,8 92,1 34,7 4,2 96,3 36,3 4,6 100,8 38,1
STONE 2
SAND 1 42,5 16,0 5,3 47,8 18,0 5,8 53,6 20,2 6,3 59,9 22,6
SAND 2
ADMIXTURE 0,0 0,0 0,0 0,0
Total 182,6 77,4 191,7 80,8 201,7 84,6 212,6 88,67

SLUMP mm mm mm 50 mm

Comments:
Mix done by: Date:
Cubes marked:

Figure 58: 15% metakaolin mix design

75
CONCRETE MIX DESIGN
CLIENT: STUDENT No 213506133 PROJECT:Dissertation
REQUIREMENTS: STRENGTH: 40 MPa SLUMP: 40-70 mm W/C: 0,61

MATERIAL TYPE AND SOURCE SIZE RD: LBD CBD FM K VALUES HAND MOD HEAVY
[mm] [kg/m^3] [kg/m^3} STONE COMP VIBR VIBR
CEMENT NPC PRO - CEMIIB-S 42.5N 3,1 9,5 0,75 0,8 1
METAKAOLIN HIGH REACTIVITY - K40 2,6 13,2 0,84 0,9 1,05
STONE 1 TILLITE 19 2,65 1360 1446 19,0 0,94 1 1,05
STONE 2 26,5 1 1,06 1,1
SAND 1 UMGENI RIVER SAND 2,65 1320 1400 2,30 FOR CBD [kg/m^3} 1446
SAND 2 STONE 19
PERCENTAGE METAKAOLIN Dosage: 20 % mass SELECTED K 1
1 m^3 (1000 l) NOTE: kg/RD = litres STONE REQD [kg] 1113,42

STONE REQUIRED [from chart using stone size and FM of sand] 1113,42 kg

MIX 1 MIX 2 MIX 3 MIX 4


MATERIAL kg litre kg litre kg litre kg litre
WATER 240 240 230 230 220 220 210 210
CEMENT 315 102 302 97 289 93 275 89
METAKAOLIN 79 30 75 29 72 28 69 26
STONE 1 1113 420 1113 420 1113 420 1113 420
STONE 2 0 0 0 0 0 0 0 0
SAND 1 551 208 592 224 633 239 674 255
SAND 2 0 0 0 0 0 0 0 0
ADMIXTURE 0 ml 0 0 0
TOTAL 2298 1000 2313 1000 2327 1000 2342 1000
FACTOR mix size/1000 x (w ater mix 1)/(w ater mix X)
0,0792 0,0792 0,0827 0,0864 0,0906

LAB MIX
MIX 1 MIX 2 MIX 3 MIX 4
MATERIAL kg Litre Add kg kg Litre Add kg kg Litre Add kg kg Litre
WATER 19,0 19,0 0,0 19,0 19,0 0,0 19,0 19,0 0,0 19,0 19,0
CEMENT 24,9 8,0 0,0 24,9 8,0 0,0 24,9 8,0 0,0 24,9 8,0
METAKAOLIN 6,2 6,2 6,2 6,2
STONE 1 88,2 33,3 3,8 92,1 34,7 4,2 96,3 36,3 4,6 100,8 38,1
STONE 2
SAND 1 43,7 16,5 5,3 49,0 18,5 5,8 54,8 20,7 6,3 61,1 23,0
SAND 2
ADMIXTURE 0,0 0,0 0,0 0,0
Total 182,1 76,8 191,2 80,3 201,2 84,0 212,1 88,16

SLUMP mm mm mm 42 mm

Comments:
Mix done by: Date:
Cubes marked:

Figure 59: 20% metakaolin mix design

76
A.3. Metakaolin Pricing

Figure 60: Metakaolin pricing from Serina Trading Company

77
APPENDIX B: Tabulated results and raw data
B.1. Fineness modulus by sieve analysis

Table 16: Sieve analysis of fine aggregate

Sieve sizes Mass Percentage Cumulative Percentage


(mm) Retained (g) retained (%) retained (%) Passing (%)
4.75 5 1 1 99
2.36 16 3.2 4.2 95.8
1.18 46 9.2 13.4 86.6
0.6 107 21.4 34.8 65.2
0.3 214 42.8 77.6 22.4
0.15 108 21.6 99.2 0.8
Passing 0.15 1 0.2 100 0
Totals 100 230.2
FM = cumulative % retained/100 = 2.3

B.2. Fresh concrete properties

Table 17: Table of fresh concrete properties

0,54 W/B W/B ratio used for Slump for Temperature


Slump 30-70mm slump W/B used
0% 70 0,54 70 23
5% 60 0,54 60 21
10% 32 0,57 55 19
15% 13 0,58 50 17
20% 4 0,61 42 17

B.3. Mechanical properties

Table 18: Compression and flexural strengths

Compression strengths (MPa)


7 day 28 day 56 day
0%MK 22,76 33,49 43,42
5%MK 22,49 42,43 46,63
10%MK 27,76 41,21 49,80
15%MK 25,00 36,79 41,72
20%MK 19,69 36,33 41,22
Flexural Strengths (MPa)
7 day 28 day 56 day
0%MK 3,6 4,4 4,61
5%MK 3,74 4,76 5,01
10%MK 3,83 4,66 4,74
15%MK 3,81 4,56 4,66
20%MK 3,37 4,56 4,94

78
Table 19: 7 day loading tests

Compressive loading (kN) - 7 day


Sample 0% 5% 10% 15% 20%
1 493,7 495,3 669,2 588 459,4
2 558,2 500,5 591,5 576,1 440,5
CUBE 3 484,6 522,4 612,8 523,1 429
AVG 512,17 506,07 624,5 562,4 443,0
% Increase -1,19 21,93 9,81 -13,51
Compressive loading (kN) - 7 day
1 12,2 13 12,7 12,8 12,5
2 12,3 11,8 13,1 12,7 10,3
BEAM 3 11,5 12,6 12,5 12,6 10,9
AVG 12,00 12,47 12,8 12,7 11,2
% Increase 3,89 6,39 5,83 -6,39

Table 20: 28 day loading tests

Compressive Loading (kN) - 28 day


Sample 0% 5% 10% 15% 20%
1 753,9 964,8 901,4 761,3 847
2 826,7 942,7 977,3 847,7 860,8
CUBE 3 680,2 956,2 903,2 874,3 744,4
AVG 753,60 954,57 927,30 827,77 817,40
% Increase 26,67 23,05 9,84 8,47
Flexural Loading (kN) - 28 day
1 14,7 15,9 15,8 15,2 15,2
2 14,7 16,6 15,1 15,1 15,2
BEAM 3 14,6 15,1 15,7 15,3 15,2
AVG 14,67 15,87 15,53 15,20 15,20
% Increase 8,18 5,91 3,64 3,64

Table 21: 56 day loading tests

Compressive Loading (kN) - 56 day


Sample 0% 5% 10% 15% 20%
1 992,7 964,8 1104,5 953,1 941,4
2 1016,1 1103,4 1194,5 949,1 857,3
CUBE 3 922,3 1079,4 1062,7 913,7 983,8
AVG 977,03 1049,20 1120,57 938,63 927,50
% Increase 7,39 14,69 -3,93 -5,07
Flexural Loading (kN) - 28 day
1 14,5 15,6 16,2 15,8 16,7
2 15,3 17,8 15,5 15,8 16,2
BEAM 3 16,3 15,7 15
AVG 15,37 16,70 15,80 15,53 16,45
% Increase 8,68 2,82 1,08 7,05

79
Table 22: Result deviation from mean

Mechanical properties- deviation from mean


7day 1 -3,61 -2,13 7,16 4,55 3,71
CUBE 2 8,99 -1,10 -5,28 2,44 -0,56
3 -5,38 3,23 -1,87 -6,99 -3,15
7-day 1 1,7 4,3 -0,5 0,8 11,3
BEAM 2 2,5 -5,3 2,6 0,0 -8,3
3 -4,2 1,1 -2,1 -0,8 -3,0
28-day 1 0,04 1,07 -2,79 -8,03 3,62
CUBE 2 9,70 -1,24 5,39 2,41 5,31
3 -9,74 0,17 -2,60 5,62 -8,93
28-day 1 0,23 0,21 1,72 0,00 0,00
BEAM 2 0,23 4,62 -2,79 -0,66 0,00
3 -0,45 -4,83 1,07 0,66 0,00
58-day 1 1,60 -8,04 -1,43 1,54 1,50
CUBE 2 4,00 5,17 6,60 1,12 -7,57
3 -5,60 2,88 -5,16 -2,66 6,07
58-day 1 -5,64 -6,59 2,53 1,72 1,52
BEAM 2 -0,43 6,59 -1,90 1,72 -1,52
3 6,07 -0,63 -3,43

Table 23: Actual vs NPC estimated strengths

0,54 0,54 0,57 0,59 0,61


(0MK) (5MK) (10MK) (15MK) (20MK)
7 day - Actual Strength 22,76 22,49 27,76 25,00 19,69
7 day - Estimated Min. 26,14 26,14 23,42 21,61 20,08
7 day - Estimated mean 29,34 29,34 26,52 24,64 23,06
28 day - Actual Strength 33,49 42,43 41,21 36,79 36,33
28 day - Estimated Min. 40,2 40,2 37,3 35,37 33,53
28 day - Estimated mean 45,2 45,2 42,3 40,37 38,53

ACTUAL VS NPC STRENGTHS


COMPRESSION STRENGTH

50,00
40,00
(Mpa)

30,00
20,00
10,00
0,00
0,54 (0MK) 0,54 (5MK) 0,57 (10MK) 0,59 (15MK) 0,61 (20MK)

7 day - Actual Strength 7 day - Estimated Minimum 7 day - Estimated Average


28 day - Actual Strength 28 day - Estimated Minimum 28 day - Estimated Average

Figure 61: Actual vs NPC estimated strengths

80
B.5. Mass, density and absorption

Table 24: Mass, density and absorption data

Satur Unsatu Mean Density W/B Wate Perce


ated rated Specimen mass (g) Mass (kg/m3) Ratio r ntage
mass mass 1 2 3 (g) Absor absor
(g) (g) ption ption
0% 8039 7998 8038 8002 8095 8045 2384 0,54 41 0,51
5% 8081 8042 8085 8096 8120 8100 2400 0,54 39 0,48
10% 8066 8024 7980 8096 7950 8009 2373 0,57 42 0,52
15% 7955 7915 7958 7970 8035 7988 2367 0,58 40 0,50
20% 7858 7814 7753 7978 7993 7908 2343 0,614 44 0,56

AVERAGE DENSITY
2420 0,62
2400

WATER-BINDER RATIO
2400 2384 0,6
MASS (g)

2380 2373 0,58


2367
2360 2343 0,56
2340 0,54
2320 0,52
2300 0,5
0%MK 5%MK 10%MK 15%MK 20%MK

Density W/B Ratio

Figure 62: Average density

AVERAGE MASS
8200
8100
8100 8045
MASS (g)

8009
7988
8000
7908
7900

7800

0%MK 5%MK 10%MK 15%MK 20%MK


PERCENTAGE METAKAOLIN

Figure 63: Average mass

81
B.6. Porosiscope results

Table 25: Air/Water permeability data

Porosiscope results
Air Permeability
Time (s) AER (s/ml) Category
0% MK 217 53,599 Fair
5% MK 857 211,679 Good
10% MK > 1000 > 250 Excellent
15% MK > 1000 > 250 Excellent
20% MK > 1000 > 250 Excellent
Water Permeability
Time (s) WAR (103 s/ml) Category
0% MK 227 22700 Fair
5% MK 493 49300 Good
10% MK 560 56000 Good
15% MK 589 58900 Good
20% MK 619 61900 Good

WATER ABSORPTION RATE (WAR)


700
619
589
600 560
493
500
WAR (103 s/ml)

400

300
227
200

100

0
0% MK 5% MK 10% MK 15% MK 20% MK

Figure 64: Water absorption rate

82
B.6. Water Sorptivity results

Table 26: Water sorptivity data

Mass (g) vs Time (min)


Specimen 0 3 5 7 9 12 16 20 25
0%MK 1 261.70 262,50 262,60 262,70 262,75 262,80 262,90 262,96 263,00
2 269,00 269,60 269,67 269,70 269,77 269,79 269,87 269,90 269,94
3 272,40 273,16 273,20 273,25 273,27 273,32 273,35 273,38 273,44
4 267,50 268,10 268,15 268,20 268,26 268,30 268,32 268,38 268,46

5%MK 1 264,70 265,40 265,43 265,50 265,53 265,57 265,60 265,66 265,70
2 265,70 266,60 266,63 266,70 266,73 266,75 266,80 266,88 266,90
3 266,30 266,90 266,98 267,00 267,05 267,10 267,14 267,18 267,22
4 257,20 258,10 258,20 258,26 258,30 258,35 258,40 258,47 258,50

10%MK 1 266,60 267,10 267,15 267,18 267,20 267,23 267,26 267,30 267,32
2 262,40 263,00 263,02 263,03 263,05 263,05 263,07 263,09 263,10
3 261,50 262,40 262,45 262,48 262,51 262,54 262,57 262,59 262,62
4 261,50 262,28 262,29 262,30 262,33 262,35 262,37 262,39 262,41

15%MK 1 256,60 257,20 257,22 257,24 257,25 257,27 257,30 257,31 257,33
2 255,00 255,90 255,95 256,00 256,03 256,09 256,14 256,18 256,20
3 258,80 259,50 259,53 259,57 259,60 259,63 259,65 259,68 259,70
4 251,20 252,00 252,05 252,11 252,19 252,22 252,26 252,32 252,37

20%MK 1 256,40 257,00 257,08 257,12 257,14 257,19 257,22 257,26 257,30
2 256,00 256,60 256,66 256,70 256,73 256,79 256,82 256,86 256,90
3 254,00 254,90 254,93 254,95 254,97 254,98 255,03 255,06 255,10
4 258,10 258,90 258,92 258,97 259,00 259,07 259,10 259,16 259,20

Table 27: Water sorptivity results

Water Sorptivity (mm/√hr) W/B


0%MK 4,86 0,54
5%MK 4,45 0,54
10%MK 2,26 0,57
15%MK 3,57 0,58
20%MK 3,78 0,61

83
Water sorptivity summary 0%

Specimen 1 2 3 4
diameter 70 70 70 70
thickness 30 30 30 30
Time (min) Mass (g)
0 261,70 269,00 272,40 267,50
3 262,50 269,60 273,16 268,10
5 262,60 269,67 273,20 268,15
7 262,70 269,70 273,25 268,20
9 262,75 269,77 273,27 268,26
12 262,80 269,79 273,32 268,30
16 262,90 269,87 273,35 268,32
20 262,96 269,90 273,38 268,38
25 263,00 269,94 273,44 268,46
Msv (g) 266,934 274,38 277,848 272,85

Mwti (g) 5,234 5,38 5,448 5,35


area (mm^2) 3848,45 3848,45 3848,45 3848,45
d (mm) 30 30 30 30
pw (g/mm^3) 0,001 0,001 0,001 0,001
n 4,533427 4,659885 4,718783 4,6339
F 1,1896 0,8123 0,6435 0,8147
S 6,818494 4,529554 3,543502 4,568411

AVG WS 0% 4,86499 mm/√hr

Figure 65: Water sorptivity summary- O%MK

Mwt vs √hr Mwt vs √hr


1,6 1,2

1,4
1
1,2
0,8
1

0,8 0,6
y = 1,1896x + 0,5666
0,6 R² = 0,9812 0,4 y = 0,8123x + 0,432
0,4 R² = 0,9851
0,2
0,2

0 0
0 0,2 0,4 0,6 0,8 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7

Mwt vs √hr Mwt vs √hr


1,2
1,2

1
1

0,8 0,8

0,6 0,6
y = 0,6435x + 0,6205 y = 0,8147x + 0,4222
R² = 0,9926 R² = 0,9842
0,4 0,4

0,2 0,2

0 0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7

Figure 66: 0% MK - Mwt vs √hr

84
Water sorptivity summary 5%

Specimen 1 2 3 4
diameter 70 70 70 70
thickness 30 30 30 30
Time (min) Mass (g)
0 264,70 265,70 266,30 257,20
3 265,40 266,60 266,90 258,10
5 265,43 266,63 266,98 258,20
7 265,50 266,70 267,00 258,26
9 265,53 266,73 267,05 258,30
12 265,57 266,75 267,10 258,35
16 265,60 266,80 267,14 258,40
20 265,66 266,88 267,18 258,47
25 265,70 266,90 267,22 258,50
Msv (g) 269,99 271,01 271,63 262,34

Mwti (g) 5,294 5,314 5,326 5,144


area (mm^2) 3848,45 3848,45 3848,45 3848,45
d (mm) 30 30 30 30
pw (g/mm^3) 0,001 0,001 0,001 0,001
n 4,585396 4,602719 4,613113 4,455473
F 0,7182 0,7358 0,7425 0,9242
S 4,06989 4,153933 4,182313 5,389969

AVG WS 5% 4,449026 mm/√hr

Figure 67: Water sorptivity summary- 5%MK

Figure 68: 5% MK - Mwt vs √hr

85
Water sorptivity summary 10%

Specimen 1 2 3 4
diameter 70 70 70 70
thickness 30 30 30 30
Time (min) Mass (g)
0 266,60 262,40 261,50 261,50
3 267,10 263,00 262,40 262,28
5 267,15 263,02 262,45 262,29
7 267,18 263,03 262,48 262,30
9 267,20 263,05 262,51 262,33
12 267,23 263,05 262,54 262,35
16 267,26 263,07 262,57 262,37
20 267,30 263,09 262,59 262,39
25 267,32 263,10 262,62 262,41
Msv (g) 271,93 267,65 266,73 266,73

Mwti (g) 5,332 5,248 5,23 5,23


area (mm^2) 3848,45 3848,45 3848,45 3848,45
d (mm) 30 30 30 30
pw (g/mm^3) 0,001 0,001 0,001 0,001
n 4,61831 4,545553 4,529962 4,529962
F 0,513 0,2346 0,5074 0,3283
S 2,886347 1,341082 2,910516 1,883174

AVG WS 10% 2,25528 mm/√hr

Figure 69: Water sorptivity summary- 10%MK

Mwt vs √hr Mwt vs √hr


0,8 0,72
0,7 0,7
0,6
0,68
0,5
0,66
0,4 y = 0,513x + 0,3977
R² = 0,9907 0,64
0,3 y = 0,2346x + 0,5508
R² = 0,9833
0,62
0,2

0,1 0,6

0 0,58
0 0,2 0,4 0,6 0,8 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7

Mwt vs √hr Mwt vs √hr


1,2 0,92
0,9
1
0,88
0,8 0,86
y = 0,3283x + 0,6993
0,6 y = 0,5074x + 0,8026 0,84
R² = 0,9857
R² = 0,9828 0,82
0,4
0,8
0,2 0,78

0 0,76
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7

Figure 70: 10% MK - Mwt vs √hr

86
Water sorptivity summary 15%

Specimen 1 2 3 4
diameter 70 70 70 70
thickness 30 30 30 30
Time (min) Mass (g)
0 256,60 255,00 258,80 251,20
3 257,20 255,90 259,50 252,00
5 257,22 255,95 259,53 252,05
7 257,24 256,00 259,57 252,11
9 257,25 256,03 259,60 252,19
12 257,27 256,09 259,63 252,22
16 257,30 256,14 259,65 252,26
20 257,31 256,18 259,68 252,32
25 257,33 256,20 259,70 252,37
Msv (g) 261,73 260,10 263,98 256,22

Mwti (g) 5,132 5,1 5,176 5,024


area (mm^2) 3848,45 3848,45 3848,45 3848,45
d (mm) 30 30 30 30
pw (g/mm^3) 0,001 0,001 0,001 0,001
n 4,44508 4,417363 4,48319 4,351535
F 0,3131 0,7457 0,4824 0,8817
S 1,830281 4,386471 2,795981 5,264928

AVG WS 15% 3,569415 mm/√hr

Figure 71: Water sorptivity summary- 15%MK

Mwt vs √hr Mwt vs √hr


0,8 1,4

0,7 1,2
0,6 1
0,5
0,8
0,4 y = 0,3131x + 0,5308
R² = 0,9946 0,6
y = 0,7457x + 0,7417
0,3
R² = 0,9866
0,4
0,2

0,1 0,2

0 0
0 0,2 0,4 0,6 0,8 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7

Mwt vs √hr Mwt vs √hr


1,4
1
0,9 1,2
0,8
1
0,7
0,6 0,8
y = 0,8817x + 0,6122
0,5 y = 0,4824x + 0,6008
0,6 R² = 0,9824
0,4 R² = 0,9807

0,3 0,4
0,2 0,2
0,1
0 0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7

Figure 72: 15% MK - Mwt vs √hr

87
Water sorptivity summary 20%

Specimen 1 2 3 4
diameter 70 70 70 70
thickness 30 30 30 30
Time (min) Mass (g)
0 256,40 256,00 254,00 258,10
3 257,00 256,60 254,90 258,90
5 257,08 256,66 254,93 258,92
7 257,12 256,70 254,95 258,97
9 257,14 256,73 254,97 259,00
12 257,19 256,79 254,98 259,07
16 257,22 256,82 255,03 259,10
20 257,26 256,86 255,06 259,16
25 257,30 256,90 255,10 259,20
Msv (g) 261,53 261,12 259,08 263,26

Mwti (g) 5,128 5,12 5,08 5,162


area (mm^2) 3848,45 3848,45 3848,45 3848,45
d (mm) 30 30 30 30
pw (g/mm^3) 0,001 0,001 0,001 0,001
n 4,441615 4,434686 4,40004 4,471064
F 0,6709 0,7043 0,4642 0,7536
S 3,924922 4,126758 2,741339 4,379698

AVG WS 20% 3,793179 mm/√hr

Figure 73: Water sorptivity summary- 20%MK

Mwt vs √hr Mwt vs √hr


1 1
0,9 0,9
0,8 0,8
0,7 0,7
0,6 0,6
0,5 y = 0,6709x + 0,4763 0,5
0,4 R² = 0,9807 0,4 y = 0,7043x + 0,4557
0,3 R² = 0,9909
0,3
0,2 0,2
0,1 0,1
0 0
0 0,2 0,4 0,6 0,8 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7

Mwt vs √hr Mwt vs √hr


1,2 1,2

1 1

0,8 0,8

y = 0,7536x + 0,6171
0,6 y = 0,4642x + 0,7911 0,6
R² = 0,9896
R² = 0,9849
0,4 0,4

0,2 0,2

0 0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7

Figure 74: 20% MK - Mwt vs √hr

88
APPENDIX C: Pictures from research

Figure 75: KG K40 high Figure 76: Fine and coarse aggregate for the mix
reactivity metakaolin

Figure 77: Weighing material Figure 78: Tilting mixing drum

Figure 79: Slump test Figure 80: Moulds on vibrating table

89
Figure 81: Fresh concrete in cube mould Figure 82: Fresh concrete in beam mould

Figure 83: Wet controlled curing Figure 84: Wet and damp curing

After all samples were cured in the curing room shown in figure 64 for 5 days, the cubes
were placed in a water bath and beams were damp cured as seen in figure 65 for the
remaining curing times.

Figure 85: Compression test Figure 86: Abnormal failure of


cube

90
Figure 87: Coring from cubes

Figure 88: Drying discs in oven Figure 89: Mixing Calcium


hydroxide solution

Figure 90: Slices for SEM imaging

91
Figure 91: 0% Metakaolin cube

Figure 92: 10% Metakaolin cube

As seen in figure 72 and 73, the inclusion of metakaolin produces an improved finish with
smooth faces, sharp edges, reduces pores/voids and a lighter coloured concrete.

92
Figure 93: 0% and 10% Metakaolin beams

Figure 94: Cubes in water bath

As seen in figure 74 and 75, the inclusion of metakaolin produced concrete that became
lighter with an increase in the metakaolin content.

93
APPENDIX D: ECSA Outcomes

94

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