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RHEOLOGICAL AND MECHANICAL BEHAVIOR OF MICROFINE CEMENT-BASED GROUTS by Marc-André Langevin Department of Civil Engineering and Applied Mechanics McGiIi University Montréal, Canada November 1993 A THESIS SUBMITIED TO THE FACUL TV OF GRADUATE STIJOIES AND RESEARCH IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF MASTER OF ENGINEERING © Copyright 1993 by Marc-André Langevin
Transcript
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RHEOLOGICAL AND MECHANICAL BEHAVIOR

OF MICROFINE CEMENT-BASED GROUTS

by

Marc-André Langevin

Department of Civil Engineering and Applied Mechanics

McGiIi University

Montréal, Canada

November 1993

A THESIS SUBMITIED TO THE FACUL TV OF GRADUATE STIJOIES

AND RESEARCH IN PARTIAL FULFILLMENT OF THE REQUIREMENTS

FOR THE DEGREE OF MASTER OF ENGINEERING

© Copyright 1993 by Marc-André Langevin

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ABSTRAcr

Some of the hydrauhc structures in Québp,c are faced with serious

cracking problerns lOir reJSOi1S such as age, freeze-thaw cycles, alkali­

aggregate reactivity (J\AR), wel' 'I1g-drying cycles, excessive applied loads,

etc. One way of (epairing these cracks is to inject them with a liquid/resln

which solidifies with time. Portlémd cement, epoxy resins, polymers and

polyurEllhanes ,are the materials normally used 10 strengthen or seal concrete

structures but recentlv a new type of (;eml~nt ~;JI!~d "microfine cement",

manufactured in Europe and Japan, has become available on the Canadian

market.

Vrliry little information is available so far about the rheological and

rnechanical chamGt(~ristics of these new prodiJets, especially for the harsh

climatlc conditions enc:ountered in the northem parts of Ouébec and other

parts of Canada. \lePI few results at ,an ambient temperaturc of 20°C are

supplied by the manufacturers.

The primary objective of this e)(perimental research program was,

therefore, to define the characteristics of microfine cement-ba~ied grouts at

different ambient temperé:ltures using thel following parameters:

• Ten cements: 2 Portland cements (Type 10 and Type 30) were

used as reference cements, 1 Portland with 8% of siliC:8 fume, and!

7 microfine cements: Microcern 1650SR, Micfocl9m 900, Lanko 737,

MC500, Spinor A 12, Spinor A 16 and Spinor E12.

• Thirteen characteristics: 3 rheological

bleeding, sE~tting tlme) and 10 mechanical

pmperties (viscosity,

properties (orain size,

modulus of elasticity and Poisson's ratio, compressive strength,

indirect tEmsile strength, bond strength (direct tensile),

shrinkage/expansion, ultrasonic pulse velocity, water permeability

and leachecl Vlater analysis, and miGrostructural characteristics .

• Three ternperatures: 4°C, 10°C and 20°C.

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• Eight water/cement ratios (0.4:1, 0.5:1, 0.6:1,0.8:1,1.0:1,1.2:1,

1.5:1 and 2.0:1/.

• Other parameters: different types and amounts of admixtures,

mixing times and mixlng speeds.

The study revealed that:

• Temperature variations have a strong influence on grouts' setting

time and some mechanlc31 characteristics (compressive strength,

modulus of elasticity, Poisson's ratio, etc.).

• The variation of graut water/cement ratios is important for both

rheological and mechanical behavior; high W IC ratios lead to

stability problems (high bleeding), which results in an effective W IC

ratio which is not the same as the ratio recorded dw'ing mlxing.

• Superplasticizers are needed to imprave the fluidity (viscosity) of

microfine cement-based grouts :n order to achieve the same degree

of workability as the ordinary PCJrtland cements, but they increase

the graut setting time .

• Both mixing time and mixing speed (in the range tested) have

minimal effect on the rheological characteristics of the grouts .

Il

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RÉSUMÉ

Au Québec, certaines structures hydrauliques en béton sont

confrontées à des problèmes de fissuration dont plusieurs facteurs (âges,

cycles gel-dégels, réaction alcali-granulat, charges structurales, retrait au

séchage, variation de la température, etc.) peuvent être responsables.

L'injection des fissures par un produit liquide qui se solidifie avec le temps

est une méthode très utilisée par les ingénieur(e)s et responsables.

Des produits comme le ciment Portland, "époxyde, les polymères et

les polyuréthannes sont normalement utilisés lors d'une injection afin

d'étanchées ou de consolider les structures de béton. Récemment, un

nouveau type de ciment appelé "ciment microfin" est apparu sur le marché

canadien. Ces ciments sont manufacturés par différents fabricants

européens et japonais .

Une recherche bibliographique a permis de constater que très peu

d'informations sont disponibies sur les caractéristiques rhéologiques et

physico-mécaniques des ciments microfins, en particulier pour des

conditions climatiques sévères telles que rencontrées dans le nord du

Québec et du Canada. Seuls quelques résultats à la température ambiante

(200 C) sont fournis par les manufacturiers des ciments microfins.

Le but premier de cette étude est donc de déterminer les diverses

caractéristiques rhéologiques et physico-mécaniques des coulis à base de

ciment microfin testés à différentes températures. Voici les différents

paramètres de cette étude:

• Dix ciments: 2 ciments Portland (Type 10 et Type 30) servant

comme ciments de références, 1 ciment Portland Type 10 avec

8% de fumée de silice, et 7 ciments microfins (Microcem 650SR,

MicrocE..'l1 900, Lanko 737, MC500, Spinor A 12, Spinor Al 6 et

Spinor E12).

iii

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------ --- - -----------------

• Treize caractéristiques: 3 dA type rhéologiques (viscosité,

stabilité et temps de prise) et 10 de type physico-mJcaniques

(granulométrie, module d'élasticité et coefficient de Poissor"

résistance à la compression simple, résistance à la traction

indirecte, adhérence, retrait/expansion, vitesses soniques.

perméabilité à l'eau, résistance au lessivage, étude

microstructurale) .

• Trois températures: 4oC, 100C et 200C.

• Huit rapports E/C massiques (0,4: 1, 0,5: 1, 0,6: 1, 0,8: 1, 1,0: 1,

1 , 2: 1, 1, 5: 1 et 2, 0: 1 ) .

• Autres paramètres à l'étude: les effets des différents types

d'adjuvants, de la durée et de la vitesse de malaxage sur les

caractéristiques rhéologiques.

L'étude a montré les points suivants:

• La variation de température affecte grandement le temps de prise

ainsi que certaines caractéristiques physico-mécaniques (fc', E,

adhérence et le retrait/expansion) des coulis de ciment microfin.

• La variation des rapports E/C initiaux est un paramètre qui af~cte

énormément les caractéristiques rhéologiques et physico-

mécaniques des coulis. Les rapports eau/ciment élevés entraînent

des problèmes de stabilité (volume de ciment en suspension). Ce

qui résulte-en un rapport eau/ciment final qui est différent de

celui lors du malaxage (initial).

• Les superplastifiants améliorent la fluidité et la viscosité des

coulis à base de ciment, mais augmentent leur temps de prise.

• Les effets de la durée et de la vitesse de malaxage (à partir d'un

certain temps et vitesse) sont minimes sur les caractéristiques

rhéologiques des coulis .

iv

l

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i

ACKNOWLEDGMENTS

The author would like to thank Professor M.S. Mirza, Department of

Civil Engineering and Applied Mechanics, McGili University, for his guidance,

advises and encouragement during thls pioject.

The author would also wishes to express his sincere appreciation and

gratitude to Dr. J. Mirza, researcher at the Direction Technologies de

Production et Matériaux (DPTM), Hydro-Québec, who acted as the internai

advisor for this research program.

A word nf gratitude goe5 also to Dr. K. Saleh, group leader at the

Direction Technologies de Production et Matériaux (DPTM), Hydro-Québec,

for his valuable advice during the whole project .

Would like to thank T. Mnif, doctoral student at Université de

Sherbrooke, for his active participation during the experimental phase

(mechanical tests) done at Sherbrooke.

The 8uthors owe thanks to Dr. B. Durand and A. Watier, researcher

and technician respectively, at the Direction Technologies de Production et

Matériaux (DPTM), Hydro-Québec, for their assistance during the use of the

laboratory facilities at l'Institut de Recherche en Électricité du Québec

(IREQ), Hydro-Québec .

v

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TABLE OF CONTENTS

ABSTRACT

RÉSUMÉ

ACKNOWLEDGMENTS

LIST OF TABLES

LIST or FIGURES

LIST OF PHOTOS

SYMBOLS

ABBREVIATIONS

1. INTRODUCTION

2. SCOPE OF STUDY

3. BACKGROUND

3.1 Causes of cracks in concrete

3.2 Inspection and determination of cracking

3.3 Crack repair methods

3.3.1 Chemical grouting

3.3.1.1 Sodium silicate formulations

3.3.1.2 Acrylnmide grouts

3.3.1.2 Lignosulfonate grouts

3.3.1.4 Phenoplast grouts

3.3.1.5 Aminoplat grouts

3.3.1.6 Water reactive materials

3.3.1.7 Organic polvmers

VI

iii

v

xi

xiii

xvii

xviii

xix

1

3

5

6

7

8

9

9

10

10

11

1 1

11

12

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• 3.3.2 Cement grouting 12

3.3.2.1 General procedure 13

3.3.2.2 Equlpment 14

4. MATERIALS 18 4. 1 Review of previous research work 18 4.2 Cements 22

4.2.1 Hydr~lllic cements 23 4.2.1.1 Hydraulic limes 23

4.2.1.2 Natural cements 24 4.2.1.3 Portland cements 24

4.2.1.4 Blended Portland cements 30 4.2.1.5 Special cements 32

4.2.2 Non-hydraulic cements 33 4.3 Admixtures 33

4.3.1 Chemical ad mixtures 33 4.3.1.1 AcceleralOrs 34

• 4.3.1.2 Retarders 34 4.3.1.3 Air-entraining agents 34 4.3.1.4 Water reducers 35 4.3.1.5 Superplasticizers 39 4.3.1.6 Other admixtures 41

4.3.2 Mineral admixtures 41 4.3.2.1 Natural materials 42 4.3.2.2 By-product materials 43

5. CHARACTEAISTICS OF GROUTS 46 5. 1 Viscosity 46

5.1.1 Newtonian flow behavior 47 5.1.2 Non-Newtonian flow behavior 48

5.1.2.1 Pseudoplastic behavior 49 5.1.2.2 Dilatant behavior 49 5.1.2.3 Bingham behavior 50

5.2 Thixotropy and rheopecty 52 • 5.3 Bleeding (stability) 53 5.4 Factors affecting rheological properties of grouts 56

VII

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6. EXPERIMENTAL PROGRAM

6. 1 Materials used

6.1.1 Cements

6.1 .1.1 Chemical composition

6.1.1.2 Grain size analysis

6.1.2 Superplastlcizers

6.1.3 Anti-washJut agents

6.2 Grout and speClrtlen preparation

6.3 Rheological tests

6.3.1 Viscosity

6.3.2 Bleeding (stability)

6.3.3 Setting tlme

6.4 Mechanical tests

6.4.1 Modulus of elastlcity and Poisson's ratio

6.4.2 Compressive strength

6.4.3 Indirect tensile (splitting) strength

6.4.4 Bond strength

6.4.5 Shrinkage/expansion

6.4.6 Ultrasonic pulse velocity

6.4.7 Permeabllity and leached water analysls

6.4.8 Microstructural characteristlcs

7. EXPERIMENTAL RESUl TS AND DISCUSSION

7.1 Determination of effective W le ratios

7.2 Effect of W le ratio

7.2.1 Fresh graut characteristics

7.2.2 Hardened grout characteristlcs

7.3 Effect of temperature

7.3.1 Fresh graut characteristics

7.3.2 Hardened grout characteristics

7.4 Effect of chemical ad mixtures

7.4.1 Superplasticlzers

7.4.2 Anti-washout agents

7.5 Effect of mixing

7.5.1 Mixing time

7.5.2 Mixing speed

VIIi

59

59

60

60

62

67

67

67

71

71

72

73

76

76

78

78

79

80

81

83

85

86

86

87

87

100

118

118

122

128

128

140

144

144

147

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• 8. SUMMARY AND CONCLUSIONS 151

8.1 Summary 151

8.2 Conclusions 152

8.3 Future work 153

REFERENCES 155

APPENDIX A: Viscosity calibration curves A-1

APPENDIX B: Viscosity tables B-1

APPENDIX C: Suspension volumes tables C-1

APPENDIX D: Setting time tables 0-1

APPENDIX E: Modulus of elasticity and Poisson's ratio tables E-1

• APPENDIX F: Compressive strength tables F-1

APPENOiX G: Bond strength (tensile) tables G-1

APPENDIX H: Ultrasonic pulse velocities and dynamic elastic

constants H-1

APPENDIX 1: Viscosity results 1-1

APf"=NDIX J: Volumes in suspension results J-1

APPENDIX K: Setting time results K-1

APPENDIX L: Modulus of elasticity results L-1

APPENDIX M: Compressive strength results M-1

• APPENDIX N: Shrinkage/expansion results N-1

ix

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APPENDIX 0: Ultrasonic pulse velocity results

APPENDIX P: Mixing time effects: Rheological properties

APPENDIX Q: Mixing speeds effects: Rheological properties

x

0-1

P-1

Q-1

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• LIST OF TABLES

Table 4-1 Particle sile classification 23

Table 4-2 Symbols for chemical oxides and compounds 25

Table 4-3 Portland cement types 26

Table 4-4 Compound characteristics 26

Table 4-5 Blended Portland cement types 31

Table 4-6 Mineral admixtures 41

Table 4-7 Natural pOllolan classification 43

Table 6-1 Cements used 59

• Table 6~2 Cement types 60

Table 6-3 Chemical composition (% weight) of cements 61

Table 6-4 Bogue composition (% weight) of cements 61

Table 6-5 Cem«1nt grain size distribution 64

Table 6-6 Cements' mean and maximum grain size and specifie area 64

Table 6-7 SuperplasUcizers used 67

Table 6-8 Weiqht of cement and water vs. initial W/C ratio ta obtain 5.5lof grout 69

Table 6-9 Characteristics tested at 4°C, 10°C and 20°C 70

Table 6-10 Permeability of cement paste (W IC = O. 7) with the progress ot hydration 84

Table 6-11 Permeability of cement paste and different rocks 84

• Table 7-1 Effective W/C ratios vs. initial W/C ratios 86

Xl

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• Table 7-2 Absolute vis~osity of different liquids 118

Table 7-3 Grout internai temperature variation vs. surrounding tempe rature 119

Table 7-4 Relative viscosity for differen: rT'ixing times taken just after mixing 144

Table 7-5 Relative viscosity for different mixing times 60 min after mixing 145

Table 7-6 Volume in suspension for different mixing times 120 min after mixing 145

Table 7-7 Initial setting time for different mixing times 146

Table 7-8 Final setting time for different mixing times 146

Table 7-9 Relative viscosity for different mixing speeds taken just after mixing 148

• Table 7-10 Relative viscosity for different mixing speeds 60 min after mixing 148

Table 7-11 Volume in suspension for different mixing speeds 120 min after mixing 149

Table 7-12 Initial setting time for different mixing speeds 150

Table 7-13 Final setting time for different mixing speeds 150

• XII

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• LIST OF FIGURES

Fig. 3-1 Causes of concrete cracking 6

Fig. 3-2 Schematic of injection equipments 14

Fig. 4-1 Applicat!ons of microfine cement~based grouts 19

Fig. 4-2 Cement classification rnatrix 22

Fig. 4-3 Sequence of hydration of Portland cern,ent 28

Fig. 4-4 Typical air-entraining surfactant formula 35

Fig. 4-5 Mechanism of air-entrain ment agents 35

Fig. 4-6 Improvements of concrete characteristics with water reducers 36

• Fig. 4-7 Typical unit of lignosulfonate molecule 37

Fig. 4-8 Typical hydroxycarboxylic acids 37

Fig. 4-9 Typical hydroxylated polymers 38

Fig. 4-10 Polar chains absorbed on cement particle surface 38

Fig. 4-11 Representation of defloculation process by ""ater reducers 39

Fig. 4-12 Typical superplasticizer molecules 40

Fig. 5-1 Newtonian flow model 47

Fig. 5-2 Newtonian flow behavior 48

Fig. 5-3 Newtonian velocity profile (pipe flow) 48

Fig. 5-4 Pseudoplastic flow behavior 49

Fig. 5-5 Dilatant flow behavior 49 • Fig. 5-6 Bingham flow behavior 50

XIII

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• Fig. 5-7 Bingham velocity profile (pipE! flow) 51

Fig. 5-8 AIJparent and plastic viscosities of Bingham fluid 51

Fig. 5-9 Bingham thixotropic and rhelO~lectic behavior 52

Fig. 5-10 Thixotropy and 1 heopecty viscosities vs. time 53

Fig. 5-11 Bleed water (%) for various initial W/C ratios (volume) 54

Fig. 5-12 Example of effective W/C ratios (settled grouts) 55

Fig. 6-' Grout penetration stopped by a) plug (bridge) and b) grain clumps 63

Fig. 6-2 Particle size distribution for dilfferent cements 65

Fig. 6-3 Crack types and suggested model for bleeding test 74

Fig. 6-4 Schematic diagram of ultrasonic apparatus 82

• Fig. 7-1 Relative viscosity just after nlixing at 20 0 e 89

Fig. 7-2 Relative viscosity (at 60 min) at 20°C 90

Fig. 7-3 Suspension volume after 120 rnin at 20 0 e 93

Fig. 7-4 Final suspensiof'l volume at 20°C 94

Fig. 7-5 Initial setting time at 20 0 e 97

Fig. 7-6 ~.nal setting time at 20°C 98

Fig. 7-7 Modulus of elasticity vs. initial w/e ratio at 20°C 101

Fig. 7-8 Modulus of elasticity vs. effective W/C ratio at 20 0 e 102

Fig. 7-9 Compressive strength vs. initial W le ratio at 20 0 e 104

Fig. 7-10 Compressive strength vs. effective W/C ratio at 20°C 105

Fig. 7 .. 11 Bond tensile strength at 20 0 e 107

• Fig. 7-12 Shrinkage/expansion at a temperature of 20 0 e and a relative humidity of 100% 109

XIV

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------------------ --- ----

• Fig. 7-13 Shrinkage/expansion at a tempe rature of 20°C and a relative humidity less than 30% 110

Fig. 7-14 Shear (transversal) wave speec~ at 20°C 112

Fig. 7-15 Compression (longitudinal) wave speeds at 20°C 113

Fig. 7-16 Dynamic modulus of elasticity at :zooC 114

Fig. 7-17 Rate of he:)t liberation 121

Fig. 7-18 Modulus of elê}sticity vs. curing tomperature 124

Fig. 7-19 Compressive strength vs. cu ring temperature 126

fig. 7-20 Relative viscosity of Type 10 cement with a napththalene-based SP at 20°C '129

Fig. 7-21 Relative viscosity of Type 10 cement with a melamine-based SP at 20°C 129

• Fig. 7-22 Relative viscosity of Spinor A 12 MC with a melamine-based SP at 20°C 1130

Fig. 7-23 Relative viscos;ty of Spinor A 16 and E12 MCs with a melamine-based SP at 2üoC 130

Fig. 7-24 Relative viscosity of MC500+SP and Lanko 737 MCs at 20°C 131

Fig. 7-25 Suspension volume of Type 10 cement with a niapththalene-based SP at 20°C 133

Fig. 7-26 Suspension volume of Type 10 cement with a melamine-based SP at 20°C 134

Fig. 7-27 Suspension volume of Spinor Al 6 and El 2 MCs with a melamine-based SP at 20°C 134

Fig. 7-28 Suspension volume of Spinor A 12 MC with a melamine-based SP at 20 ° C 135

• Fig. 7-29 Initial setting time of Type 10 cement with a napththalene-based SP at 20°C 136

xv

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'. Fig. 7-30 Final setting time of Type 10 cement with a napththalene-based SP at 20°C 136

Fig. 7-31 Initial setting time of Type 10 cement with a n.dlamine-based SP at 20°C 137

Fig. 7-32 Final setting time of Type 10 cement with a melamine-based SP at 20°C 137

Fig. 7-33 Initial setting time of MC500 + SP, Lanko 737 and Spinor E12 + SP(melaminel at 20°C 138

Fig. 7-34 Final setting time of MC500·:- SP, Lanka 737 and Spinor E 12 + SP(melamine) at 20°C 138

Fig. 7-35 Initial setting time of Spinor A 12 and A 16 with a melamine-based SP at 20°C 139

Fig. 7-36 Final setting time of Spinor A 12 and A 16 with a melamine-based SP at 20 0 e 139

• Fig. 7-37 Reliative viscosity of Type 10 wÎth AWAs at 20 0 e 140

Fig. 7-38 Sunpension volume of Type 10 with AWAs at 20 0 e 141

Fig. 7-39 Ini1ial setting time of Type 10 with AWAs at 20 0 e 142

Fig. 7-40 Final setting time of Type 10 with AWAs at 20 0 e 143

xvi

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• LIST OF PHOTOS

Photo 6-1 Brookfield viscometer 72

Photo 6-2 Bleeding test 73

Photo 6-3 Vicat apparatus 75

Photo 6-4 Hydraulic compression machi"e 77

Photo 6-5 Tensile strength machine 80

Photo 7-1 Type 10 cement with an initial W/C ratio of 0.8 (3500X) 116

Photo 7-2 Type 30 cement with an initial W/C ratio of 0.8 (3500X) 116

Photo 7-3 Microcem 650SR cement with an initial W IC ratio of 0.8 (llOOX) 117

• Photo 7-4 MC500 + SP cement with an initial W IC ratio of 0.8 (2200X) 117

• xvii

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E:

f " c'

v:

~:

~m:

SYMBOLS

Modulus of elasticity (Pa)

Dynamic modulus of elgsticity (Pa)

Compressive Strength (MPa)

Poisson's ratio

Dynamic Poisson's ratio

Viscosity (cps)

Microns

XVIII

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• ABBREVIATIONS

AWA: Anti-Washout Agent

A12: Microfine Cement Spinor A 12

A16: Microfine Cement Spinor A 16

050: Cement Mean Grain Size (/lm)

0100: Cement Maximal Grain Size (~m)

Eî2: Microfine Cement Spinor E12

L737: Microfine Cement Lanko 737

MC: Microfine Cement

MC500: Microfirle Cement MC500 • r-iPM: Revolution per minute

SEM: Scanning Electron Microscope

SF: Silica Fume

SP: Superplasticizer

T10: Portland Cement Type 10

T10SF: Portland Cement Type 10 with Silica Fume

T30 Portland Cement Type 30

W/C: Water /Cement Ratio (weight)

650SR: Microfine Cement Microcem 650SR

900: Microfine Cement Microcem 900

• XIX

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CHAPTER 1

INTRODUCTION

Cracking is a problem that occurs most frequently during the building

and operation of concrete hydraulic structures. Major causes of cracking

include design errors, drying s,dinkage, temperature variations, freeze-thaw

cycles, aging of the structures, chemical reactions such as alkali-aggregate

reactions (AAR), subsidence of the foundations, strains and stresses,

displacement, etc. [1,2J.

Hydro-power utilities such as dams, generating stations and other

si:ructures built of concrete are assets that the owners are anxious to

piOtect and maintain in good operating conditions. The repair technique

frequently consists of injecting mors or less viscous products into the

cracks, depending on their width and depth, and the amblent conditions

such as temperature, humidity, etc.

The materials used for injection are based on normal Portland cernent,

epoxy, polyurethane, or polyester [31. However, observations and the results

of various tests have revealed that microcracks injected with Portland

cement-based grouts are not completely filled; it is only the macrocracks

(opening > 0.5 mm) that are filled by this method [4, 51. It is therefore not

very efficient to inject microcracks with normal Portland cement, and the

engineers need to use other products based on epoxy, polyurethane,

polymers or microfine cements (MC).

Epoxy-, polymer- and polyurethane-based products have tW:l major

drawbacks: their considerably higher cost compared with that of the

Portland cement and the difference between their thermal expansion

coefficients and that of concrete. Also, low temperatures increase the

viscosity of these prOdL:0ts, making it difficult to in je ct deep into cracks and

their setting times. Sorne of them also have poor bondmg in moist

r.nvironments (I.e. cracks) or in those with a very wide opening [61.

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Microfine cements, which are similar to the basic material of the

structure to be repaired (same thermal expansion coefficient, etc. 1,

therefore, offer an interesting alternative to the chemical products, although

it is important to test them at the sa me tempe ratures as those prevalent in the structures in Canada.

This study presents the results of rheological alld mechanical

behavior of different microfine cements subjected to the various tests at these different temperatures .

2

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CHAPTER 2

SCOPE OF STUDY

There are various products available for injecting the cracks in

structures damaged by the harsh climatic conditions such as those ln

Québec. These structures are exposed to severe thermal variations, which

affect the efficiency of some products. The advent of new microfille

cements in the mid 1980s increased the range of alternative products for

repairing the cracks in these structures. However, these cements are made

by European and Japan manufacturers who are very reluctant to piOvlde full

rheological and mechanical data, although thls is essential for analyzmg the

behavior of the grouts prepared using these microflne cements. When they

do supply information, they limit themselves to providing the values

determined at ambient temperatures of around 20°C and rarely provide any

values at lower temperatures. Also, very few publications and sClentlfic

reports are available in the literature.

It IS, therefore, important to determine the rheological and mechanical

characteristics of microfine cement-based grouts at temperatures which are

more typical of the Canadian climate. However, thls work must be preceded

by a laboratory study which will supply the results for application in the

field.

The main objectives of this research project are listed below:

• A complete bibliographic study of mlcrofine cements, tests

performed, characterlstics, injection purposes, case studies, etc.

• Completion of 13 series of tests in accordance wlth the existing

standards (ASTM and CSA) at different temperatures (4'JC,

100 C and 200 C) to study the behavior of mlcroflne cement­

based grouts in the fresh and hardened states (rheological and

mechanical properties respectively): grain size analysis

(fineness), viscosity, bleeding (stabihty), settln9 tlme, modulus

3

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of elasticitv and Poisson's ratio, compressive strength, indirect

tensile (splitting) strength, bond strength (tensile), shrinkage

and expansion, ultrasonic pulse velocities, water permeability

(and chemical analvsis of leached water), and microstructural cha racteristics.

• Evaluation of the performance and behavior of microfine

cements bV studying the results of the different test series at

the three selected temperatures by modifying the water/cement (W/C) ratio.

• Verification of the degree to which parameters such as the

mixing time and rate, and the addition of ad mixtures such as

superplasticizers (SP) and anti-washout agents (AWA) have any

influence on the rheological characteristics of a cement-based grouts .

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CHAPTER 3

BACKGROUND

When the function of a structure is impaired by cracking, suitable

actions need to be undertaken to improve either the strength, the stiffness,

the durability, or (to a lesser degree) the appearance of the structure and

enhance these characteristics to an acceptable level.

The first step before proceeding to a repair is to evaluate the causes

of cracking and microcracking. Then, a survey should be undertaken to

determine the extent and locations of cracks. Finally, if repairs are needed,

different available techniques should be examined, and the best one for the

specifie job must be chosen. This study will concentrate only on repair of

cracks or microcracks in concrete structure, especially dams, using injection

of microfine cements-based grouts [2] .

Injecting a liquid (which solidifies with time) into a crack or microcrack

for repair purposes has become one of the most commonly used crack repair

methods over the pa st few years. As mentioned previously, there are many

cases where injection is useful for repairing dams and other concrete

structures [7] :

• When the overall integrity of the dam needs improvement.

• Wh en the flow of water causes serious deterioration of the

structure by dissolution of the concrete and joint erosion.

• If freeze-thaw cycles cause the concrete to fracture and

disintegrate the concrete.

• If the water increases the AARs.

• Should vertical pressure threaten the structure.

• For seepage control (through or under a dam).

• When the amount of water lost affects the volume of water

• stored in the basin.

5

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3.1 Causes of cracks in concrete

Most hydraulic structures are built mainly of concrete as their basic

material. With age and/or other factors [1, 2] the concrete develops cracks;

a fairly large number of possible repair techniques are exist and are available

for repairing these cracks. The causes of cracking (Fig. 3-1) depend on the

degree of hardness attained by concrete.

Cracking during construction

1

Thermal effects

Un favorable non-linear

temperature gradient wlthm mass concrate

1

Coohng of concrete from the maximum temperature durmg hydrEltlon to Its fmal

stable temperature

CRACKS

1

Chemlcal reaetlons

1 ln service cracks

1

Volume changes

1 MOlsture Foundatlon content settlement

Drymg Shrmkage

stress tram

Applled loads

Seasonal temperature variations

1 1 1 1 1 1 Alkall Sulfate

aggregate attack reactlons

Mg(OH)2 Ca(OH)2 Freeze/ Expanslon/ Wet/dry tha\,' contraction

Fig. 3-1 Causes of conerete cracking [1]

Cracking of plastic concrete are principally due to:

• Plastic shrinkage cracking of exposed surfaces (from lack of

moisture).

• Settlement cracking.

• Subsidence after initial placement of the conerete .

6

1

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Cracking of hardened concrete occurs principally due to:

• Drying shrinkage.

• Chemical reactions (AAR, sulfate attacks, deicing salts, etc).

• Thermal stresses (heating-cooling cycles).

• Freeze-thaw cycles.

• Drying-wetting cycles.

• Corrosion of reinforcement.

• Poor construction practices.

• Construction overloads.

• Errors in design and detailing.

• Application of external applied loads.

3.2 Inspection and determination of cracking

A good maintenance program requires a detailed inspection of the

structure at regular intervals. There are three different ways of inspecting a

structure: a visual inspection, nondestructive and destructive tests on the

concrete. The following is a brief summary for each type of inspection, as

given in by the ACI committee 224 [2]:

• Visual inspection

This is the easiest form of inspection and ail routine maintenance

programs should include it. The information (location and width of

cracks) are marked on a sketch of the structure along with appropriate

photographs. Crack widths can be measured with the help of a crack

comparator (up to 0.025 mm) and crack movements can also be

monitored with mechanical instrument or, more accurately, with LVOTs

and data acquisition systems.

• Non destructive testing

These tests are used to determine the presence of internai cracks,

voids and their depth. An easy method is to use a hammer to hit the

surface to identify planar cracking under it. Another technique is to use

7

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------------------- ._----_.

an ultrasonic equipment: a mechanical pulse is transmitted through the

concrete member and it is received using another transducer. This

informations is used to calculate the pulse velocity. The higher the pulse

velocity, the better is the concrete quality. Presence of cracks slows

down the pulse velocity which can be recorded with an oscilloscope.

Finally, radiography is another type of nondestructive test that may be

used ta identify the crack location in the members.

• Destructive testing

Cores can be taken fram the different members. It is then easy to

locate and measure the width of the cracks or microcracks in the

structure. Chemical tests may also be used to determine if there is an

excess of chlorides in the specimens, which can accentuate the corrosion

of the reinforcement. The cores can also be tested to determine their

compressive strength.

3.3 Crack repair methods

Several methods exist to repair successfully cracks in a concrete

structure. Depending on the nature, the extent and the location of the

cracks, the best method should be chosen by the engineers. The following

are the ma st used methods in the industry [2]:

• Routing and sealing.

• Stitching.

• Adding conventional reinforcement.

• Adding prestressing reinforcement.

• Drilling and plugging.

• Flexible sealing.

• Grl..'luting (cement- and chemical-based).

• Drypacking.

• Crack arresting .

Sections 3.3.1 and 3.3.2 will focus only on the grouting of cracks in

concrete structure with chemical- or cement-based grouts.

8

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3.3.1 Chemical grouting

Grouting with chemical products has been used successfullv to repair

cracks in many concrete structures such as bridges, dams, tunnels, buildings

and ta consolidate soils or rock foundations. The first patent for a chemical

grout (sodium silicate and coagulant) was issued in 1886 to Jeziorsky, a

European scientist [6]. But the modern era of chemical grouting is fairlv

recent and dates from the early 1950s.

The main advantage of these products in the rehabilitation of concrete

structures is that the chernical grouts can be injected lOto microcracks as

narrow as 0.05 mm. Depending on the nature of the crack (active or

dc."mant), several products are available on the market. When the crack is

still active, the product aets as a sealant and it is flexible enough ta allow

the crack to function as a joint. Thus in this case, the crack is not

consolidated, but it is simply sealed or made watertight. On the other hand,

if the crack is dormant, a chemical grout which solidifies over a period of

time (as a cement-based grout) is needed to fill and consolidate the crack

[2].

There are so many chemical grouts available that it is difficult to set a

standard classification system. The early systems (in the 1960s) were based

01" the mcchanical properties of the grouts. They can also be listed based on

their chemical components. This latter's classification is used here and

chemical families are listed below.

3.3.1.1 Sodium silicate formulations

Sodium silicate is maliufactured as an aqueous (colloidal) solution.

When it is mixed with a salt (CaCI2). a chemical reaction takes place ar.d a

gel is formed. The mix between the two products can be implemented in one

or two phases, but the best results are obtained when the two phase

approach is used (injecting the solution of sodium silicate in the ground or

crack and then injecting the calcium chloride). The main advantage of this

method is that the gel is hard (for a chemical grout, but weak compared to a

cernent grout). The disadvantages are that the solution has a high viscosity,

9

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which will not penetrate fine cracks, and it is impossible to have a complete

reaction between the two liquids injected.

A new approach is to use a combination between sodium silicate

(basic) and a bicarbonate mixture (weak acid). When a diluted sodium

silicate solution is mixed with an acid solution, silicate precipitates and forms

a gel by neutralization after a certain time [6J. This i'ormulation has the

advantage that its low viscosity, it can penetrate microcracks. However,

there are many disadvantages such as its very low strength; the setting time

(control gel time) can be very long and shrinkage can become a problem

with time. Therefore, this chemical grout should not be used to consolidate

cracks, but only to waterproof them.

3.3.1.2 Acrylamide grauts

These grouts are a mixture of two organic monomers (in the liquid

phase): 95% of acrylamide which polymerize (at ambient temperature) into

long molecular chains and 5% of cross-lin king agent (methylenebis­

acrylamide) which binds the chains together. The final product is a solid

plastic which becomes a tough and durable product but it has a low

compressive strength. The advantages of these chemical grouts are that

they have a very low viscosity (near water); they resist chemical attacks and

can soak into dry concrete, filling the cracks and microcracks at the same

time. The major drawbacks are their high degree of toxicity and flammability,

their poor strength, hey cannot be injected in a moist cracks (will not mix

with water) and they may suffer volume changes with time [6]. Therefore,

these type of grouts cannot be used to consolidate cracks and microcracks

in a concrete structure.

3.3.1.3 Lignosulfonate grouts

The lignosulfonates are a waste liquor (by-product) of the wood

processing industries (paper mills). The chemistry of chrome lignin grout is

very complex and consist of lignosulfonates and a hexavalent chromium

compound. The viscosity and the gel setting 'LÏme vary with the

concentration of solids used in the mixture. The main advantages of

10

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lignosulfonates grouts are that they have a low viscosity and they are

relatively inexpensive. But they do not have adequate compressive strength

needed to consolidate a crack and they are highly toxic [6]. As the previous

products, ligosulfonates are not recommended to consolidate cracks and

microcracks.

3.3.1.4 Phenoplast grouts

These resins are polycondensates fram the reaction of a phenol on an

aldehyde. They set only at high temperature over a wide pH range (used in

the oil-well industry). In order to use them at ambient temperature, an acid

medium is needed. The other option, if acidity is not desirable, is to use

resorcinol (other type of phenol) with a formaldehyde. The compressive

strength of such a grout increas'3s significantly with the resornicol

concentration, but the gel setting time decreases rapidly. As for many

chemical grouts, phenoplast grouts are very toxic to the environment [6].

Phenoplast cannot be considered to cracks' consolidation due to their weak

compressive strength.

3.3.1.5 Aminoplast grouts

Aminoplast resins are made of urea and formaldehyde, or other

polymers. The major drawbacks are that the reaction can be accomplished

only at high tempe rature and require an acid environment to complete the

reaction such as phenoplast resins. This type of grout also gives low

strength compared to a normal cement-based grout (thus not used for

cracks' consolidation) buy they have a low viscosity which permits them to

be injected in fine cracks or soils, and they are relatively inexpensive but

they are also toxic and corrosive and cannot be used in areas of high pH [61.

These chemical grouts are not recommended for cracks' consolidation.

3.3.1.6 Water reactive materials

These materials form a gel, or a foam or polymerize when they come

in contact with water. Thus, polyethylene, polyvinyl, CCA are polymers that

have very little viscosity values and can fill cracks and microcracks in

Il

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concrete as narrow as 0.05 mm. These foam type grouts have the

advantages of being applicable in moist environ ment (excess moisture

available) and they have wide limits of control gel time. But, these mate rials

have following disadvantages: a high degree of ski Il is needed when these

grouts are injected, they have a low compressive stiength (thus they are

used to seal cracks, not to consolidate them) and they must not dry out in

service [2, 6J.

3.3.1.7 Organic polyrners

Epoxy resins, polyesters and polyurethanes are organic polymers that

have excellent mechanical characteristics. In fact, their compressive strength

is the highest of ail chemical grouts manufactured and they, therefore, can

be used to consolidate cracks and microcracks. Their viscosity is slightly

higher than the other chemical grouts but they still can be injected in very

fine cracks (up to 0.05 mm). Finally, these organic polymers are very

expensive, they have problems to set at low temperatures (and they set too

rapidly at high temperature), they require high skilled personnel to

manipulate them, they have a high coefficient of thermal expansion

(compared to concrete), they have a bonding problem in a moist

environment, anà they can suffer volume changes over time [2, 6J.

3.3.2 Cement grouting

This type of grouting, normally \!Vith normal Portland cements, is used

mainly to repair wide cracks in concrete structure. It is understood from

several sources that the pioneers of Portland cement-based grouting are

Brunei (1838), Kinipple (1856) or Hawksley (1876) [4, 6]. Since the advent

of Portland cement, there was no major breakthrough on the material itself.

The recent coming of microfine cements provides a wider choice of

materials, compared with the chemical grouts wh"n the grout is to be

injected into microcracks.

The choice of the cement is based on the crack width, the

environ mental conditions (presence of sulfate, etc.) and economical reasons:

12

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• If the crack is wide, Portland cement grout should be used and it

may even contain sand.

• If the crack is fine (opening < 0.5 mm), microfine cements

grouts should be used instead of a normal Portland cement

(avoid blockinq the crack prematurely).

• If sulfate dttack is a problem, Type 50 Portland cement grout

(normal or fine ground) should be used.

• Finally, grouting with Portland cement is cheaper than chemical­

or MC-based products.

Various ad mixtures may also be rnixed with the grout (see Chapter 4)

to improve the different properties such as viscosity, bleeding (stability),

setting time, strength etc. The most used admixtures are the

superplasticizers, . ~tarders, silica fume, fly ash, blast-furnaced slags, etc.

3.3.2.1 General procedure

The general grouting procedure can be simplified to the following;

mixing the grout, storing it for short time until it is needed and pumping it

into the crack or holes. In the case of crack repair, the procedure with a

cement-based grout given by the ACI Committee 224 [2] may be

summarized as follows:

• Cleaning the concrete along the crack.

• Drilling grout holes if necessary.

• Installing built-up seats (grout nipples) at intervals along the

length of the crack.

• Sealing the crack between the seats with a cement paint, sealant

or grout.

• Flushing the crack to clean it and test the seal. This is also

performed to estimate the grout volume and the pressure

needed.

• Grout the whole area.

• After the crack is filled, the pressure should be maintained for

several minutes to insure good penetration.

13

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3.3.2.2 Equipment

The injection process has improved over the last 90 years with the

de"plopment of new technologies and equipment. Three basic components

forma part of every arrangement: the mixer, the agitator and the pump (see

Fig. 3-2). Houlsby [4] specifies that the most important component is the

mixer because it affects greatly the quality of the grout.

11111. __

Fig. 3-2 Schematic of injection equipments [4]

14

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• Mixers

A good mixer should produce a cement- or MC-based grout which

have the following characteristics:

Cement grains are separate from each oth13r (no flocs or clumps).

Each cement grain is wetted and surrounded by a thin film a

water.

The grout is uniform.

Minimum sedimentation or bleeding.

1- High-speed. high-shear mixers

The above characteristics can be obtain when the materials Icement,

water and admixtures) are mixed with a high-speed, high-shear mixer

equipped with a vortex drum. The speed maintained by such a mixer

has ta be at least 1500 rpm for a minimum mixing time of 15

seconds. The speed is obtain by the use of a hlgh-speed rotor which

produces violent turbulence and hlgh shearing action [4]. The

functions of the vortex drum are to receive the materials and to act as

a centrifugai separator. The most used brands of mixer by the

injection inc1ustry are the Colcrete, the Cernix, the Chemgrout and the

Hany [4].

2- Combined mixers

The combined mixers are less efficient than the high-speed. high-shear

mixers. These mixers have a slower speed between 700 and 1000

rpm and the rotor is located in the base of the drum. A pump is used

to circulate the grout back to the drum or directly to the cracks, if it 15

a small job. A mixing time of 3 minutes is needed to obtain an

acceptable grout quality. The combined mixers can produce uniform

grouts but the w~tting and the separation of cement grains is not

always obtained because of the lack of high shear property .

15

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3- RQller mixers

The roller mixers are also less efficient than the high-speed-shear

mixers. Vertical rollers are used for mixing a cement-based grout and

revolve toward each other to mix the different materials. These mixers

must be IQcated ta a higher point than the agitators since the grout is

discharged by gravity.

4- Paddle mixers

These are the cheapest type of mixers available but also very popular.

Paddles or a propeller revolve at a slow rate (100 to 700 rpm) in a

drum. This low shear (and energy) mixing takes approximately 5

minutes and produce a low quality grout.

• Agitators

The functions of the agitators are to store and to keep the graut

continuously stirred until lt is pumped into the cracks. They are also

useful to verify the quality of the grout coming from the mixer. A

simple tank with paddles revolvin3 at low speed (approximately 100

rpm) are the main items of an agitator .

• Pumps

The pumps are machines that take the grout from the agitator tank

and inject it into the cracks or the grout holes. There are two types of

pumps.

,- Helical rotor Dumps

These pumps are in the "no-valves" category. They are equipped with

a helical steel rotor which revolves slowly at 300 rpm inside a softer

stator. The pressure output is steady and depends on the length or

the rotor and its speed. The common brand used for grouting is the

Mono or Moyno [4].

16

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2- Piston pumDs

Pistons pumps used for grouting have either two, four or six pistons

moving in close-fitting cylinders (like a car). In the case of a 2-valves

pump, when one piston moves to expel grout, the other one make a

suction on the other side to suck in grout tram the agitator tank.

Valves are used to control the outflow port white the inflow takes

place.

• Other components

The other pieces needed for a complet ion injection kit are the control

valves (diaphragm, bail and plug cocks), the pressure gauges, the

packers, the washout gears, the circulation lines (pipes) .

17

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CHAPTER 4

MATERIALS

This chapter reviews the research work conducted on the microfine

cements (fundamental research, field test, case study if available, etc.). It

also presents a detai/ed review of the most used cementious materials and

ad mixtures (chemical and mineraI).

4.1 Review of previous research work

It should be pointed out that injection is not a new repair method, or

even one that has appeared during this century. Actually, the Romans were

the first to employ this method using a rudimentary clay-type repair material

to strengthen walls, bridges, aqueducts, etc. Pressure grouting is the

invention of a French engineer named Charles Berigny in 1S02 when he

used this technique (with a suspension of clay and lime) to repair ports'

masonry walls in Dieppe [4].

The discovery of Portland cement at the beginning of the 19th century

revolutionized the injection process. At the same time, technological

advances (injection methods, equipment, materials, etc.) enabled injection to

be extended to other purposes beyond .Ile repair of simple cracks in

structures. Nowadays it is employed for filling, sealing and strengthening

foundations and many other applications. As seen in Fig. 4-', examples

range from underground applications (repairing faults in rock, unstable soil,

etc.), grout curtains for dams, sealing of tension rods, injections in oil wells,

strengthening of foundations, underground storage depots for hazardous or

nuclear waste, etc. [S, 9].

More recently, the advent of different additives or admixtures,

especially water reducers and superplasticizers, have improved the

performance of grouts based on holding cement in suspension [10, 11].

18

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NUClEAA WASTE CONTAINMENT

NuaEAA 11~ WASTE ~

+ Grouting zona

DAMCUATAIN GAOUTING

Curtoln-grouting

HAZARDOUS WASTE PLUME STABILIZATION

FOUNDATION GAOUTING

~~~~

ConscIdaIbr groulÏng

Fig. 4-' Applications of microfine cement-based grouts [13]

Portland cements are impossible to use for injecting microcracks in

concrete with very small openings. A number of new products based on

chemical substances (organic/resins such as epoxy, polyurethane, polyester,

etc.) appeared on the market toward the end of the 1950s [12]. Sorne of

these chemical substances, however, had a major handicap; they were not

environmentally friendly to the soil, the ground water table, etc., or

sometimes incompatible (bond strength, thermal expansion coefficient,

moisture, etc.) with certain materials such as con crete [2, 6]. Other

drawbacks that cannot be ignored are resin shrinkage in wide cracks, the

sometimes infinite setting times at low temperatures and the high cost

compared to Portland cement .

19

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It was only after a toxic accident in Japan (early 1970s) [13], where

strengthening work was being do ne with acrylamide-based grouts in an

unstable soil, that research began in earnest into alternative materials. The

early 1980s th us saw the banned organic materials in Japan replaced by a

much safer product, microfine cements (MC) [13, 14]. Their fine grain size

allows them to be injected into fine, sandy soit or into cracks aven with very

small openings « 0.5 mm) and to achieve performance levels similar and

beyond (especially for strength) to those of chemical products [7].

Considering that microfine cements are new on the market, there is

very little information in the world apart from a few research pa pers on

fundamental research in the laboratory [3, 8, 10, 13, 16, 35] mostly at

normal temperature (approximately 200 C).

Some researchers have managed to determine a number of rheological

characteristics of microfine cement-based grouts when used with different

admixtures [10]. They concluded that:

a) The viscosity increases with larger specifie surface areas of the

cement (Blaine).

b) Addition of bentonite increases the viscosity.

c) Addition of bentonite introduces more thixotropy.

d) Addition of superplasticizers reduce the viscosity for a limited

period of time.

e) The addition of both bentonite and superplasticizers with a cement

grout improve significantly the fluidity.

Very recently, Saleh et al. [15] studied the rheological and meehanical

characteristics of microfine cement-based grouts at two different

temperatures (4°C and 20°C). This study allowed the research team to

determine the behavior of grouts in terms of variations in the W IC ratio, the

arnount of admixtures and variations in temperature. In certain cases, ranges

of the W le ratios that can be used for the injection of cracks were also

specified. However, they conclude that the most important points to

consider for the final choice of grouts are the configuration, the crack

conditions and state of the structure to be repaired.

20

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Other factors that may have an influence on the rheological

properties of cement or MC-based grouts include the mixing rate and mixing

time. Houlsby [4] suggests that "high-speed, high-shear energy" mixing

contributes positively to the quality of the grout. This has led other

researchers ta pursue the phenomenon in light of these two parameters

[1 6] . They also verified the effect of water temperature on some rheologi" al

characteristics. Their findings are as follows:

a) The type and duration of grout mixing and the water temperature

(5 oC, 20°C and 35 OC) do not affect the grout bleed rate and bleed

capacity.

b) An increase in the grout mixing time substantially increases the

viscosity (especially for low W/C ratios).

c) Decreasing the water temperature increases significantly the grout

viscosity for low W IC ratios, but has little effect on grouts with

high W/C ratios.

d) The grout setting time is hardly influenced at ail by the mixer type

(thus mixing speed) or duration .

e) A faster grout mixing rate increases the compressive strength of

hardened specimens.

f) An incre8se in the grout W/C ratio results in a decrease in the

compressive strength.

g) MC500 grouts (MC500 is a microfine cement) were generally

stronger that other cements for the same W IC ratios.

The first major studies on the use of microfine cements for injection

were related to projects designed to strengthen the soil or cracked rock

foundation. As far as the repair of concrete dams and other hydraulic works

or concrete structures is concerned, no published data seems to be

avaiJable. However, a number of manufacturers of microfine cements claim

that their products have been used for injecting cracks in dams (in Europe),

but this information could not be provided and remained confidential.

21

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4.2 Cements

Cementious materials have been used for thousand of years, from the

simple mud walls of prehistoric megalithic structures to early Greek, Roman

and Egyptian buildings and then to the advanced high-rise concrete

structures built with high performance concrete.

ln general, cement can be defined as an adhesive substances capable

of uniting fragments or masses of solid matter to a compact whole [17].

Cements can be classified as either hydraulic or non-hydraulic (see

Fig. 4-2). A hydraulic cement (e.g. hydraulic limes, pozzolan cements, slag

cements, natural cements, alumina cements, Portland cements, etc.) harden

by reacting with water and form a product which is water resistant whereas

a non-hydraulic cement (e.g. limes) usually sets and hardens (react) with air

and the final product is not fully water resistant .

Coarse

1 Hydraulic

1

Cements 1

Intermediate Microfine

1 - Hydreuhc hmes

- Naturel cements

- Portland cements

- POlzolan cements

(natural ,fly ash, blestturnece slag, etc.)

- Alumina cements

- Others

Fig. 4-2 Cement classification mat ri x

1 ] Non-hydraulic

]

Primary Classifie-ation (set & harden propertles)

Secondary Classification (gram slze)

Tertiary Classification (chamlcal components)

Hydraulic cements may further be classified as coarse, intermediate or

microfine. Thus, the basic difference between an ordinary cement and a

22

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microfine cement is their grain size. Both these cements can be 100%

Portland or composite hydraulic cements (Portland-slag or Portland­

pozzolan). Table 4-1 shows that Type 10 or Type 30 Portland cements

would be classified as "coarse" because their average grain size (050) is

higher than 1 0 ~m, whereas a cement would be "microfine" if it has a 050

valuo below 4 ~m [15, 18J. The "050" value is the particle diameter at

which 50% of the cement grains are smaller than the diameter denoted by

050. Whereas 0100 is the size such as that 100% of the particles are

smaller than the size denoted by 0100 (thus, maximum siLe).

Table 4-1 Particle size classification

Mean Maximum

Cement types particle size (050) particle size (01001

(Ilm) (Ilm)

Coarse 050 > 10 0100 > 70

Intermediate 4 < 050 ~ 10 20 < 0100 ~ 70

Microfine 050~ 4 0100 ~ 20

The fineness of the cement particles and a good partiele gradation

(particle size distribution) enhance the characteristics of the hardened grout

at any stage in the curing process [19]. On the other hand, extremely fine

grains can create drawbacks for sorne characteristics of grouts in the fresh

state such as a very short setting time and high viscosity.

4.2.1 Hydraulic cements

The following sections contain a detailed review of the main hydraulic cements and their characteristics.

4.2.1.1 Hydraulic limes

Hydraulic limes are made by burning limestones that contain a

proportion of clay at high temperature (1000 to 12000 C). The clinker

obtained after calcination contains a proportion of lime silicate, which

provide thH hydraulic properties to the cement, and a proportion of free lime

23

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------------- -----------

that forces the clinker to slake on the addition of water. The final product

consists of lime silicate and one-fourth of hydrated lime which, by the

presence of alumina and silica compounds, hardens slowly when mixed with

water.

4.2.1.2 Natural cements

Natural cements are hydraulic cements produced by calcining a natural

mixture of calcereous and argillaceous substances at a temperature below

the sintering point and finely grinding them [17]. These cements are in a

group between hydraulic limes and normal Portland cements.

They are used less and less and many countries stopped manufacturing

them because their strength is much smaller than those of Portland cements.

They can be used when the expected stresses encountered are low or if

weight or mass is more important than strength [20].

4.2.1.3 Portland cements

Portland cements are one of the most used material for construction

purposes in the world today. When Portland cement is mixed with water, a

paste is formed and can be used from aesthetic touches on a building to a

grout used for injection. The use of sand or very fine aggregates results in a

mortar that can be used for layi'lg bricks and other masonry purposes.

Addition of coarse aggregates leads to a durable material named concrete

which can be used in many types of structural members (such as slabs,

walls, columns, etc.', structures (dams, bridges, highways, etc.' and for

other purposes (foundations, footings, etc.).

Technological advances in other parallel activities, such as minerai and

chemical admixtures, now permit to produce high performance concrete that

can sustain compressive stresses up to 138 MPa [21].

The CSA Standard CAN3-A5-M83 and the ASTM Standard C150

define Portland cement as a hydraulic cement prepared by pulverizing clinker

consisting of hydraulic calcium silicates, usually containing one or more of

24

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the forms of hydrated calcium sulfate (gypsum) as an interground addition.

The following symbols (Table 4-2) are used throughout thîs study to express

the individual oxides and clinker compounds.

Table 4-2 Symbols for chemical oxides and compounds

Oxide Chamieal Formula Symbol

Lime CaO C

Slilca SIO~ S

Alumina AI,O'.! A

Iron oXlde Fe ,0_'.1 F

Magnesium oXlde MgO M

Suif ur tnoxloe SO't S Water H,_O H

Compound ChamicalF ormula Symbol

Tncalclum sIlicate 3CaO'510? C'.IS

Dlcalclum sIlicate 2Cao 5107 C2S

Tncalclum aluminate 3CaO'AI,O~ C~A

Tetracalclum alumlOofemte 4CaO'AI,01'Fe?01 C,4AF

Hvdrated lime Ca(OHI? CH

Anhydrite CaSO,,- CS

Gypsum CaSO,,-'2 H70 CSH,

Calcite CaCO'.! cë

Portland cements are regrouped in 5 different categories depending on

the proportion of the following chemical compounds (see Table 4-3):

tricalcium silicate (C3S), dicalcium silicate (C2S), tricalcium aluminate (C3A)

and tetracalcium aluminoferrite (C4AF) [22]. Each of these compounds have

different properties with regards to strength, hydration rate and heat

liberation during the hydration reaction (Table 4-4).

The fineness of the cement will also affects the rate of hydration of

the cement grains with water. The greater is the fineness, the more rapidly

the cement will react with water and greater is the early strength

development (first 7 days) [23].

25

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Table 4-3 Portland cement types

CSA-A5 CSA Compound com-"osition (%)

designatlon

Type 10

Type 20

Type 30

Type 40

Type 50

1 ASTM C150 2 API Spec 10 3 AS 1315

Nôme

Normal

Moderate

High early strength

Low heat of hydration

Sulfate resistant

C3S C2S C3A

50 24 11

42 33 5

60 13 9

26 50 5

40 40 4

Table 4-4 Compound characteristics

Characteristics C35 C25

5trength Good Good

Rate of Fast Slow hydration Heat Medium 5mall liberated

C4AF

8

13

8

12

9

C3A

Po or

Very Fast Large

Other deslgnation

Type Il Type A 2 Class A 3 Type III Type 0 2 Class B 3 Type III l Type B 2 Class C 3 Type IV 1

ro

Type C L

Type V l

Class B 2

C4AF

Po or

slow-medium

5mall

The five standard Portland cements enumerated in the Table 4-3 have

special characteristics and are used differently depending on the job. Here is

a brief summary of their use and specifications as specified by CSA CAN3-

A5-M83 standard [22]:

,- Type 10 - Normal Portland cement

Type 10 is a general-purpose cement. For use when the special

properties specified for any other type are not required (sulfate

26

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attacks, low heat of hydration. etc.). It is used for sidewalls,

reinforced concrete buildings, bridges, railway structures, etc.

2- Type 20 - Moderate Portland cement

Type 20 is for general use, but more especially when moderate sulfate

resistance or moderate heat of hydration is needed. It is used in

drainage structures, large piers, heavy abutrnents, heavy retaining

walls, etc.

3- Type 30 - High-Early-Strength Portland cement

Type 30 is used when high early strength is desired (usually less than

a week). Thus, construction forms can be removed quickly and the

structure can be in service more rapidly. This cement aCQuires

strength more rapidly because it has a higher concentration of C3S

and has a higher specifie surface area (Blaine) [20, 23] .

4- Type 40 - Low-Heat-of-Hydration Portland cement

Type 40 is a Portland cement used when a low heat of hydration is

needed. It will develop its strength at a lower rate than Type 10

cement but it is desired when large massive concrete structures are

being built such as gravit y dams, heavy foundatior.s, etc. If

temperature is not minimized, large cracks would appear and the

structure might prove unsound (20). To minimize hydration heat,

lower concentration of C3S and C3A are used.

5- Type 50 - Sulfate-Resistant Portland cement

Type 50 is used when high sulfate resistance must be obtained. It is

used when concrete is exposed to severe sulfate action by soil or

water. It gains strength at a slower rate than Type 10 cement but its

lower concentration of C3A (less than 5%) prevents sulfate attacks .

27

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-------- ---------- -_ ... _-----

• Hydration of Portland cement

Two theories explain the mechanism of hydration between Portland

cement and water [23]. The first theory is called the "through-solution

hydration" and involves the dissolution of anhydrous compounds to their

ionic constituents, the formation of hydrates in the solution, and due to their

low s\llubility, the eventual precipitation of the hydrates from the

supersaturated solution. This theory implies a complete reorganization of the

constituents of the original compounds during the hydration of cement.

The second theory called the "solid-state hydration" of cement. It

specifies that the reactions take place directly at the surfaces (ionic mobility)

of the anhydrous cement compounds without their going into solution.

However, it appears that both theories are good: the through-solution

mechanism explain the early stages of the hydration reactions whereas the

solid-state theory characterizes the long term hydration process .

The hydration of the different compounds (aluminates and silicates) of

Portland cement involves several simultaneously reactions. But the rate of

hydration is not the same for each compound (as seen in Table 4-4) and the

sequence of hvdration may be consulted in Fig. 4-3 [24].

(a) o

• • o

Fig. 4-3 Sequence of hydration of Portland cement: al cement grains in water, 1:,1 formation of protective colloidal coatings of C-S-H gel around the grains, cl rupture of the protective coatings foilowed by secondary growth of C-S-H gel, later infiling of the microstructure by fine grained C­S-H gel and by growth of crystalline calcium oxide [241

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The following is a brief summary of the hydration process for the

major compounds:

- Hydration of the silicates

Tri- and di-calcium silicates react with water to produces a family of

calcium silicate hydrates (also called C-S-H) which are similar but

vary in the CaO:Si02 (calcium:silica) ratio f' Id combined water

[1 7]. The C-S-H gel is very poorly crystallizeJ and form a porous

solid. The stoichiometric reactions for hydrated silicates are as

follow:

(1) 2C3S + 6H ~ C3S2H3 + 3CH

(2) 2C2S + 4H ~ C3S2H3 + CH

Three major observations can be made concerning the previous

equations [23]:

1- ln equation 1, C3S2H3 (calcium silicate hydrate or C-S-H)

constitute 61 % of the hydration products whereas in equation 2,

C3S2H3 produced constitute 82% of the hydration products.

The ultimate strength of hydrated cement cornes mainly fram the

formation of calcium silicate hydrate. Thus, a cement containing

a considerable amount of C2S should attain a higher strength

with time compared with a cement with a lot of C3S,

2- If the hardened cement paste is more resistant (durable) to acid

and sulfate attacks when it has less calcium hydroxide (CH), a

cement containing a higher concentration of C2S should be more

durable than one containing a higher proportion of C3S because

the C2S hydration reaction produces less CH.

3- For a complete hydration, C2S would require 21 % of water

whereas C3S would take 24% .

29

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- Hydration of the aluminates

The first reaction that beginc; in contact with water is the one with

C3A. Crystalline hydrates (C3AHS, C4AH19 and C2AHS) are

formed very rapidly and a large amG·Jnt of heat is generated from

this hydration reaction. Therefore, gypsum is added to slow down

the reactlon in order to have sorne time to manipulate the paste.

To understand the hydration of C3A with water, the implication of

gypsum must be considered. The solubility of C3A is depressed in

the presence of hydroxyl, alkali and sdfate ions (alkalis and gypsum

go into solution quickly). Depending on the concentration of sulfate

and aluminate ions in sOlution, a precipitating crystalline product is

formed as either calcium aluminate trisulfate (ettringite) or calcium

aluminate monosulfate (C4ASH1S).

Ettringite (CSAS3H32) is the first hydrate to crystallize in normal

Portland cements (which contain about 5 % of gypsum) in the first

hour of hydration. The precipitation of ettringite contributes to

stiffening, setting and early strength of the paste. Then, after a

certain time (after the depletion of sulfate in the solution), ettringite

becomes unstable and is converted to monosulfate [23].

The ferroaluminates produce compounds which have variable

chemical compositions but structures similar to ettringite and

monosulfate. Its hydration reaction is slower than C3A.

The hydration of Portland cement is very complicated phenomenon

and cannot be explained in a few lines. More details of the hydration

process can be found in the standard textbook by Lea [17] and Mehta [23].

4.2.1.4 Blended Portland cements

These cements consist of a uniform blend of Portland cement with

either a pozzolan (fly ash, silica fume, natural pozzolan) or a granulated blast

furnace slag. A pozzolan possesses little or no cementious value but when

30

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these materials are finely grounded and are in the presence of moisture they

react chemically with calcium hydroxide to form compounds possessing

cementious properties [231. Granulated blast-furnace slag (when finely

grounded) is itself cementing and does not require calcium hydroxide to form

cementious product but it is not strong enough for structural purposes. More

details on those minerai admixtures are available in Section 4.3.2.

The CSA A362-M83 defined 3 types of blended Portland cements as

shawn in Table 4-5.

Table 4-5 Blended Portland cement types

CSA-A362 CSA Remark Other designation Name designatlon

Type lOS Portland- Slag proportIon is Type IS l

blast- between 25-70% of furnace-slag total weight

Type 10SM Slag- Slag proportIon IS Type 1 l

modifled below 25% of total Portland welght

Type 10P Portland- Pozzolan proportion IS Type IP l

Pozzolan below 40% of total welght

1 ASTM C595

The advantages of blended-Portland cements are that the amount of

heat generated is lower than that for the normal Portland cement (which is

perfect for large mass concrete volume in dams structure). They exhiblt

greater strength than normal Portland cement after 28 days and their

durability ta sulfates and acid environment is also better than normal

cements. But the disadvantages are that the early strength is smaller than

that of normal cements since the hydration reaction is slow. Also, they

require more water for a given fluidity (important in the injection process)

and they show greater shrinkage upon drying [20] .

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4.2.1.5 Special cements

Some cements exhibit special characteristics which are supposed to fill

other engineering needs which are not covered by the previous cements.

These special cements are as follow:

• Alumina cements: They have a high alumina content because they

are made by pulverizing calcium aluminate

cement clinker. The raw materials used are

limestone and bauxite. They have the following

properties: high early strength (hardening under­

taken to full strength at 48 hours instead of 28

days) even at low temperatures, excellent

refractoriness and they have superior durability

to sulfate attacks. The disadvantages are the

l05S of strength with time, especially at elevated

temperatures .

• Oil-well cements: They are slow-setting cements which are used in

the Petroleum industry wh en drilling wells.

• Expansive cements: These are hydraulic cements which expand

during the process of hydration, setting and

hardening (early hydration period). These

cements are used when shrinkage cannot be

tolerated in structural members (crack-free

pavement, slabs, etc.).

• White & colored

cements: White Portland cements are produced by the

same process as the ordinary Portland cements

except that they have a low content of iron and

manganese (which gives the grey color). Colored

cements are made by adding a chemicallY inert

pigment into the Portland cement. These

cements are used for aesthetic considerations.

32

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• Other cements: Several other special cements exist such as Ultra

high early strength cement, waterproofed

cement, hydrophobie cement, antibacterial

cement, barium cements, etc.

4.2.2 Non-hydraulic cements

The best known non-hydraulic cement is lime. This cement is made

from burning gypsum or one of the naturally occurring forms of carbonates

(such as limestonel at high temperature. The hardening process needs air

(C021 and may take several years to develop its full strength. Since it is not

used very much today, it is not pursued any further in this thesis

4.3 Admixtures

An admixture is defined as a product (usually of chemical or minerai

nature) which is added to a material or a mixture, usua!ly in small quantities,

to improve sorne of its characteristics. In the case of a cement- or MC­based grout, viscosity is one of the major characteristics needing

improvement without increasing the W/C ratio. Other characteristics that

could be improved, albeit to a lesser degree, are the bleeding rate (stability),

setting time, washout resistance (at fresh state) and the final compressive

strength.

A wide range of admixtures exist but sorne products have 1eleterious

effects on sorne of the grout characteristics. The following sections describe

the main chemical and minerai ad mixtures used for cement grouting today.

4.3.1 Chemical admixtures

There are two main types of chemical admixtures, the ones (ca lied

surfactant agents) which act on the cement-water mixture instantaneously

by influencing the surface tension of water and by adsorbing on the surface

of cement particles and the ones which break up into their ionic constituents

and affect the chemical reactions between cement and water from several

minutes to several hours after addition [23].

33

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4.3.1.1 Accelerators

Accelerating ad mixtures are normally used in cold weather to increase

the rate of hardening of cement. It permits an early strength gain as if the

temperature was normal. Different types of accelerators exist but the most

known are calcium chloride, calcium formate, aluminium chloride, alkali

hydroxide, etc. [111. Calcium chloride is the most used in North America,

but care should be takcn to reduce the corrosion risk to the reinforcement.

The effects of accelerator on the rheological characteristics of grouts

are as follow; increase in stability (reduce the bleeding rate), reduce the

setting time and increase the viscosity more rapidly after mixing.

4.3.1.2 Retarders

These ad mixtures are used to slow down the hardening and setting of

the cement-based graut, especially at high ambient temperature. They

consist generally of lignosulphonates, salts of hydracarboxlic acid, hydro­

xylated polymers, etc.

Retarders are used mainly for grouting in the oil weil industry (very

high temperature) or when the grout has to be pumped over a long distance.

It should be noted that water reducers or superplasticizers are sometimes

used instead of retarders because they have similar effects on the setting

time (increasing it) of the grouts.

4.3.1.3 Air-entraining agents

These agents are mainly used to incorporate in concrete ""'Iall air

bubbles in arder to improve its durability characteristics' (resistance to

freeze-thaw cycles and de-icing salts). It also impraves the workability of

concrete and reduces bleeding. These ad mixtures were discovered by

accident in the 1930s when engineers observed that certain roads in the

north-east states were more durable that other roads in the same area [251 .

It was concluded that the cement used had been obtained from the mills

34

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that used beef tallow (as a grinding aid) that functioned as an air-entraining

agent and improved the durability of concrete.

Air-entraining agents are made of salts of wood resins, proteinaceous

mate rials, petroleum acids, sulfonated lignin, organic salts of sulfonated

hydrocarbons and certain synthetic detergents.

ln general, these agents consist of a non-polar hydrocarbon chain with

an anionic polar grouD (Fig. 4-4). The mechanism is pretty complex and is

represented in Fig. 4-5.

Able'lc ACld

Fig. 4-4 Typical Air-entraining surfactant formula [23]

Fig. 4-5 Mechanism of air-entrain ment agents

4.3.1.4 Water reducers

The main purpose of water reducers is to produce a graut, mortar or

concrete of a given fluidity (grout) or workability (mortar and concrete) at a

lower water/cement ratio than when no admixture is added [25].

35

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Improvements are realised as shawn in Fig. 4-6. Up to 15% of water can be

remove from the mixture for a given fluidity when these admixtures are

added.

WITIWT AlJl!I XTlJ( .,.--/ "

/ LOO! WIC RATIO \ 1 HI GER !iflIfNiTH , 1 Pl{) !lm 1 LliY

IV \ HIGfR ~IMt'AII N(J J !fAT Œ\ruP.fNT

\SI/'IILM KWJSILlT'f/

~-. - //

~ 1 -

1 : i ~ 1

..... --/' "

/ \ 1 \

CIJffiU.. 1 10 SAVE œtJ(T ~ \ (])(1(TE 1 H~.1ER -œtJ(T)

\ / , / ~ __ ..... h..

:; 1 ~ '''I,j

i 1 ~ ,~~ ~ 1 ~ ~ ~ i 1 ~ ~ (,/. li! , ~' ~ - " -- ~t)~ ~ - - ~(J)

;' '" /

/SIPULAR ~ \ Nf) HIGfR

V Q)Bllm \ '\ HIGIR~ltfIΠPI{) , IEAT~ / \ /

....... / -_ .....

LOO NIC "'TlO HIGfR STTŒlH MJ DMBILITY SN'( 'GfABIUlY

SIMltAA SOOljfli. !lIW 1 L1T'f PlI) ~BllIlY

lOO~lrfJΠ~ IEAT m(MHT

( .) fau.Y A LITTU I.MR STRENGni AT EMLIEiI Na AlC) A L.I"'..! HIKR STRfNGn< AT LCt«iER AGES SHlll.D BE EXPECTED. ElCEPT ~EH Nl ACCEl.!RATlNG \ofATE.g...~ IS \.SEO: IN iHIS CASE SiilE.-mH 15 HlGElI AT EAALWI ~ UN;ER AGES.

Il

III

Fig. 4-6 Improvements of concrete characteristics with water reducers [11]

36

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Water reducers are a surfactant agent similar to the air-entraining

agents but the anionic polar group is joined to a hydrocarbon chain which

itself is polar or hydrophilic (OH groups in the chain). The typical reducers

are based on lignosulfonates (Fig. 4-7). hydroxycarboxylic acid.; (Fig. 4-81

and carbohydrates such as hydroxylated polymers (Fig. 4-91.

Fig. 4-7 Typical unit of a lignosulfonate molecule [23]

\1ale"dl C It"C dCld Tartd"c dCld \luclC dCld

_________ 1~4_~_h' ___ 12 '--4_~_h' ___ 1_"_'_5 _"6'_ FuncllonaluvOH groups

COOHgroups \folecul..lr "'~Ight

Formul. CH,COOH 1

HO-(-COOH

1 CH,C<XlH

15U

CODH 1

H-C-OH 1

HO-CH 1 CODH

CDOH 1

U-C-OH 1

HO-(-H 1

H-(-OH 1

H-(-OH 1 CDOH

Glueo",L dCld ~dllrvhc dCld HeplO",c aCld "'.hc dCld III 11 22 271 !~~I 1231 Pbl ------

Funct.onahl\ OH groups 5 COOH ,roups 1

Molecular WClghl 1%

Formula CODH 1

H-(-OH 1

HO-(-H 1

H-(-OH 1

H-(-OH 1 (H,OH

1> 1

2~1

(<XlH (ODH

60H H-t-OH

"'" 1 HO-t-H 1

H-(-OH 1

HO-(-H 1

HO-C-H 1 (H,OH

134

HO-(H-CODH 1 CH,COOH

Fig 4-8 Typical hydroxycarboxylic acids [251

37

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Fig 4-9 Typical hydroxylated po/ymers [11]

The mechanisrn of water redueers is also similar ta the air-entraining

surfactants. Mehta [23] pointed out the following situation: "When a 5mall

quantity of water is added ta the cement, without the presence of the

surfactant a well-dispersed system is not attained because, first, the water

passesses high surface tension Ihydrogen-bonded molecular structure), and

second, the cement p~rticles tend ta cluster together or form floes

(attra<.l:;ve force exists between pasitively and negatively charged edges,

corners, and surface's when crystalline minerais or compounds are finely

ground). When a sur1"actant with a hydrophilic is added ta the cement-water

system, the polar chain is adsorbed alongside the cement particle; instead of

direeting a nonpolar l:md taward water, in this case the surfactant directs a

polar end, thus lowering the surface tension of water and making the

cement particle hydrophilic IFig. 4-10). As a result of layers of water dipoles

surrounding the hydrophilic cement partieles, their floceu/ation is prevented

and a well-dispersed system is obtained (Fig. 4-11)."

_1:...-.1= 'T' fIIIolecull.,lb Anlonle Polar Gral/II J:"" J: rI ln th. Hydroeorbon Chain

Fig 4-10 Polar ehains absorbed on cement particle surface [23]

38

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B,fore AU.r

Fig 4-11 Representation of defloculation process by water reducers (23]

It should be noted that a water reducers are only effective for a specifie period of time. A water reducer will increase the setting time but,

eventually, it will phase out, as the hydration reaction takes place .

Finally, if more fluidity is needed for a given water/cement ratio,

higher dosage of water reducers is not recommended, as it may result in

unwanted effects on setting time, air content, bleeding, segregation and

hardening characteristics [11 J. Superplaticizers should then be considered as

an alternative to the normal water reducers.

4.3.1.5 Superplasticizers

Superplasticizers (SP) are a "new" class of water reducers designed to

improve mainly the viscosity of a grout (and the stability), although they

have the disadvantage of increasing the setting time. Water reducing agents

existed long before the relatively recent SPs (1970s) but the latters can

reduce the water content of a grout by up to 30% in sorne cases [11 J.

There are several types of SP on the market now but the most

commonly used consist of long-chain (high-molecular-weight anionic

surfactants) of melamine- and naphthalene-formaldehyde based products

and modified lignosulfates (Fig 4-12).

39

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SODIUM SAli Of

SODIUM IAlI DI

5UlIONAIID """AlIIII ID'MAlDIHYII ,.,

SODIUM 1IG10SUIFO!jAlI

ICI

Fig. 4-12 Typical superplaticizer molecules [11]

The superplasticizers, as water reducers, act on the grout at the

microstructural Javel. The water molecules, which are polarised, surround

the cement particles which are positively or negatively charged at their

surfaces; resulting into flocculation. The cement particles retain a certain

amount of water which can therefore no longer be used for hydration of

other particles, with the result that the grout is more viscol~s and

sedimentation of the particles takes place under the influence of gravit y,

leading to instability.

Therefore, to ensure that the grout is not too viscous, ail particles

must be hydrated but not excessively. When SP molecules are adsorbed on

cement particles, they imparts a strong negative charge which lowers the

surface tension of the surrounding water (neutralise the different electric

charges at the surface of the cement particles). It then disperses the cement

particles in the mixture, leaving the water to hydrate ail of them and reduces

the viscosity of the grout [23].

40

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4.3.1.6 Other ad mixtures

Other chemical admixtures such as anti freezing agents, damp

proofing and waterproofing agents, anti-washout agents, etc., exist on the

market; these also have a special effect on the characteristics of cement.

4.3.2 Mineral ad mixtures

As it was stated earlier, minerai admixtures are finely divided

sileceous materials which, when mixed with Portland cement, influence the

properties of concrete, mortar or grout. These materials may be classify as

follow: the natural materials (natural pozlolan) and the by-product materials

(artificial pOllolan such as fly-ash, silica fume, blast-furnace slag, etc.). The

Canadian Standard Association (CSA) classify these ad mixtures in the CSA

standard CAN3-A23.5-M82 (see Table 4-6).

Table 4-6 Mineral ad mixtures

CSA-A23.5 CSA Remark Other de sig nation Name designation

Type N Natural Product of raw or Class N l Pozzolan calcined natural

pozzolan Type F Fly-ash Low calcium fly ash Class F l

and is a product of combustion of anthracite and bituminous coals

Type C Fly -ash High calcium fly ash Class C l

and is a product of combustion of lignite and subbituminous coals

Type G Granulated These slags are Blast- weakly cementious furnace slag and pozzolan;::

Type H Granulated These slags have Blast- better cementious furnace slag properties than

Type G

1 ASTM C618

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The original definition of pozzolan is a siliceous or siliceous and

aluminous material which has almost no cementious value by its,elf but,

when finely divided and in presence of moisture, reacts chemicéJlly with

calcium hydroxide to form compounds possessing cementious v,alues (at

ordinary temperature). Thus, it needs the presence of a Portland cement

which, when mixed with water, produce calcium hydroxide (CH).

However, many fly ashes (especially Type C) and slags (Type H)

produced contain a certain percentage of CaO which is available for the

pozzolanic reaction and these ad mixtures become self-cementious to a

certain degree. These products still need an external source (Portland

cement) of calcium hydroxide to develop their full strength. Therefore, they

are not simple "pozzolans" as defined above but should be referred as

"cementious pozzolans" [23].

The benefits of these products when mixed with Portland cement are

as follow: they improve the resistance to thermal cracking (lower heat of

hydration), they increase the ultimate strength (long term), tney have better

impermeability due to pore refinement, and they have a better durability to

chemical attacks such as sulfate water and alkali-aggregate reactions.

4.3.2.1 Natural materials

Natural pozzolan are produced by crushing, grinding and size

separation of volcanic rocks and minerais. There are four types of natural

pozzolan based on the principal reactive constituent: volcanic glasses,

volcanic tuffs, calcined c!ays or shales and diatomaceous ea~1h (see Table 4-

7 for more details). These materials are classified as Type N by the standard

CSA A23.5 [22].

42

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Tabla 4-7 Natural pozzolan classification

Pozzolan Principal reactive Heat treatment constituent needed

Volcanic glasses Unaltered aluminosilicate No i glass

Volcanic tuffs Zeolite minerais Iphillipsite No and herschelite)

Calcined clays Clays and shales Ves or shales minerais Diatomaceous Organogen malerial Vas eanh (diatomite)

4.3.2.2 By-product matarials

These mate rials are secondary (waste) products produced by

industries. Several by-products are available on the markets such as fly

ashes (combustion of coa!), silica fumes (various metallurgical operations)

and granulated slag (ferrous and non-ferrous metal industries). Depending on

the by-product type, the y may need processing such as drying and

pulverization before they can be used as admixtures .

• Flyash

Fly ash is mostly produced by thermie power plant (powered coal).

The process of obtaining fly-ashes may be summarized as tollow: as

the coal is consumed in the furnaces at high temperatures, the volatile

matter and carbon are burned off and the minerai impurities (clays,

quartz, feldspar, etc.) are melt. Then, two types of ashes can be

collected: minerai matter agglomerates forming the bottom ash and

the ashes flying out (reason why they are called fly ashes) with the

flue gas stream. The tly ashes are then removed from the se gases by

electrostatic precipitators.

Fly ashes can also be divided in two groups which depend on the

calcium content of the material. The low calcium fly ashes (Type F)

contain less then 10% of analytical CaO whereas high calcium variety

contains 15 to 35% analytical CaO [11). Therefore, low calcium tly

ash is considered as a normal pozzolan whereas high calcium tly ash

43

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(Type C) is considered as a cementious pozzolan (such as granulated

blast-furnace slag)

• Blast-furnace 51ag

Blast-furnace slag is a non-metallic by-product (consisting of silicates,

aluminosilicates and other bases) of the cast iron proauction. The

chemical components of slag (in the form of crystalline melilites),

which is obtained by cooling it slowly, do not react with water at

ordinary temperature. To become a weakly cementious and pozzolanic

material, the blast-furnace slag has to be ground finely.

To obtain better cementious properties, the liquid slag has to be

rapidly quenched from a high temperature (1400-1500°CI by water or

air and water. The result is that most of the lime, magnesia, silica and

alumina are held in noncrystalline or glass y state. After being ground

finely, the admixture reacts similarly to high calcium tly ash and it is

called granulated blast-furnace slag [17, 23, 20].

CSA A23.5 divides granulated blast-furnace slag in two categories:

Type G and Type H (see Table 4-6) (22).

• Other slags

Several other slags may also show a pozzolanic or cementious

behavior. These materials are usually by-products of ferrous metal

industries such as steel, copper, nickellead, etc.

• Silica fume

Silica fume is a by-product of the induction arc fumaces in the silicon

metal and ferrosilicon alloy industries. Quartz is transformed to silicon

at very high temperature (up to 2000 0 C), and it also produces SiO

vapors which oxidize and condense (at low temperaturel to very fine

spherical particles of noncrystalline silica. The particles obtained are

44

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finer than regular fly ash and Portland cemont and it is the reason why

it is highly pozzolanic.

The CSA st~ndard A23.5 (1982) does not have specifie standards

concerning silica fumes [22] .

• ' Rice husk ash

The base mate rial for Rice husk ash is rice husks (shells produeed

during the dehusking operation of paddy rice). The husks are burned

(in open-air or in uncontrolled combustion furnace) and are

transformed into ashes which are then grounded to a very fine partiele

size in order to develop pozzolanic properties. It IS possible to obtain a

highly pozzolanic ash if it is produeed following a process developed

by Mehta and Pitt [11]

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CHAPTER 5

CHARACTERISTICS OF GROUTS

One of the main objective of this study was to verify the MC-based

grout characteristics of the grouts in fresh (rheological) and hardened states.

A cement-based graut is a mixture between a liquid (water), a solid

(hydraulic cement) and, on some occasion, chemical or minerai admixtures.

The mixture starts as a liquid but hardens over time and become a solid.

The liquid state of the grout is an important aspect to be considered

when injecting it into a crack. The grout must be sufficiently viscous for

the material ta be workable and capable of penetrating the crack but not too

viscous, so that the injection pressure does not cause any more damage to

the structure. If the grout contains tao much water, problems will eventually

appear and some rheological (bleeding, setting time) or mechanical (long­

term resistance, durability) properties will suffer [26].

This chapter will focus on the flow mechanism of grouts in Section

5.1 and 5.2 and on the grout bleeding effect in Section 5.3. Section 5.4

follows with a review of the main factors influencing the behavior of a MC­

based graut in the fresh state.

5.1 Viscosity

The American Society of Civil Engineers (ASCE) Grouting Committee

has defined the ward "viscosity" as the internai fluid resistance of a

substance which makes it resist a tendency to flow [27J. The resistance, or

friction, is apparent when a layer of fluid is made to move in relation to

another. The greater is the friction, the greater the shear force is required ta

cause movement .

46

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However, there are several types of flow behavior. They can be

classified as Newtonian or non-Newtonian depending if their viscosity is

dependent or independent of the shear rate applied [28].

5.1.1 Newtonian flow behavior

Take two parallel planes (1 and 2) of a fluid of equal area A which are

separated bya distance dx from each other. If a tangential force F (dyne) is

required ta move plane 2 with a constant speed V2 (cm/sec), then the

viscosity of this substance has poise for units. Both planes are moving in the

same direction but at different velocities V, and V2 (see Fig. 5-1). The force

F required to maintain this speed difference is proportional to the velocity

gradient [29] .

Fig 5-1 Newtonian flow model [30J

Thus, the viscosity may be written down as:

where

J.I. = (FIAI =-1-dv/dx 'Y

J.I. = viscosity (poise)

't = shear stress (dynes/cm2)

'Y = rate of shear (sec- 1 )

ln a Newtonian substance, the force required to maintain this speed

difference through the liquid is proportional ta the velocity gradient of the

liquid. Thus, a Newtonian liquid is one in which the rate of shear is directly

proportional to the tangential stress applied ta it and its viscosity is

independent of the shear rate (see Fig. 5-2).

47

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Shrear stress Rate of shear

Fig. 5-2 Newtonian flow behavior

The velocity profile of a Newtonian liquid has a parabolic form where

the velocity gradient is zero at the wall and maximum at the middle (Fig. 5-

3). The zero velocity gradient on the surface is also called the "no-slip"

condition and is caused by the viscosity of the fluid [28] .

v

Fig. 5-3 Newtonian velocity profile (pipe flow)

5.1.2 Non-Newtonian flow behavior

A non-Newtonian fluid may be defined as a substance which the

relationship t/y (shear stress/rate of shear) is not constant. The viscosity of

such substance changes as the shear rate varies. Three types of non­

Newtonian fluids exist: pseudoplastic, dilatant and Bingham (or plastic) .

48

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5.1 .2.1 Pseudoplastic bahavior

This type (Fig. 5-4) of fluid (also ca lied shear-thinningl shows a

decreasing viscosity with an increasing shear rate. Paints, emulsions and

dispersions substances show this fluid behavior.

1 Shrear stress Rite ofsh •• r

Fig. 5-4 Pseudoplastic flow behavior

5.1.2.2 Dilatant behavior

This flow behavior is also ca lied shear-thickening because the

viscosity is increasing with an increase in shear rate (see Fig. 5-5). It is a

rare phenomenon which is encountered in fluids containing high levels of

deflocculates solids such as clay slurries, sand/water mixture etc.

Shr.lr stress R.t, of sh •• r

Fig. 5-5 Dilatant flow behavior

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5.1.2.3 Bingham behavior

Bingham or plastic substances behaves like a solid under static

conditions. A minimum shearing force is needed to start the flow. When the

yield value (flow point) is reached, these substances act the same way as

Newtonian liquids (see Fig. 5-6) (29]. Cement-based grout and ketchup are

good examples showing plastic behavior.

I--l mm •• .". Shrear stress Rate of shear

Fig. 5-6 Bingham flow behavior

The viscosity (ca lied plastic viscosity for a Bingham body) equation

can be estimated as (29]:

where

Il = (t-toL y

Il = viscosity (poise)

t = shear stress (dynes/cm2)

to = initial yield stress (dynes/cm2)

y = rate of shear (sec-1)

The cement- and MC-based grouts follow the Bingham flow model.

The interparticle forces, between the solids, result in a yield stress that must

be exceeded to initiate flow as in the proposed modal. The plastie viscosity

and the yield value will influence the flow rate because they both affect the

velocity profile of the grout (see Fig. 5-7), Therefore, a plug will be

50

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formed in the zone where the stress is lower than then yield stress, and

when the pressure gradient decreases, it will grow until it reaches the wall

(of a crack) and stops the flow [10]

'ter) v (r)

Fig. 5-7 Bingham velocity profile (pipe flow) (v=velocity, ro=plug radius) [10]

Bingham and other type of non-Newtonian substance have a real or

plastic viscosity (Il) and an apparent viscosity (Ila). Thus, the viscosity

readings obtained with a viscometer will be "apparent" for a non-Newtonian

fluid and true for a Newtonian fluid. Fig. 5-8 shows the rate of shear as a

function of the shear stress for a Newtonian and a Bingham fluid.

Bon"homoen fluod

Shear stress

Fig. 5-8 Apparent and plastic viscosities of Bingham fluid

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5.2 Thixotropy and .'heopecty

Thixotropic bE!havior is a rheological characteristic found in Bingham

bodies. A substance (a grout in this case) will show an increase in the

shearing strength wlnen left undisturbed. This is then lost when it is agitated

but will regain it agêlin if a"owed to rest. Such a substance does not recover

its original rigidity immediately but it rather requires time [29].

A rheopectic flow behavior is the opposite of thixotropic flow (the

descending branch of the flow curve is to the right of the ascending branch

of the curve). Both flow behaviors are presented in Figure 5-9.

RhlOpec;tJc bod~

Shear str .. s ShNrstress

Fig. 5-9 Bingham thixotropic and rheopectic behavior [29]

These two behaviors can also be presented by a change in viscosity

with time under conditions of constant shear rate. In that case of a

thixotropic behavi()r, the fluid's viscosity decreases with time while it is

subjected to constémt shearing. The rheopectic body's viscosity will increase

with time as it is sheared at a constant rate (Fig. 5-10) .

S2

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Thlxotropy Rheopecty

Tlme

Fig. 5-10 Thixotropy and rheopecty viscosities vs time

5.3 Bleeding (stability)

The water content of a grout gives it the mobility needed for the

injection. But after the grout is in places in the cracks, the excess water

does more harm than good: it should be pointed out that the amount of

water needed to convey the graut particles exceeds the optimum amount

required for hydration of the cement particles [4]. It results in a smaller

compressive strength for the graut and it will be more permeable and less

durable.

Bleeding, also referred to as sedimentation, depends on the graut

components, i.e. the cement particles, the water and the admixtures. The

cement particles settle under the influence of gravit y (grain size and density)

as weil as the electrostatic forces present. These forces (Van der Waals and

diffusion) are due to the electric fields developed by the balanced charge of

the ions on the surface of the particles [31].

The bleeding phenomenon (see Fig. 5-11) has detrimental effect on

the final W/C ratio after the graut has been standing for a while (from a few

minutes to several hours depending on the initial W/C ratio) [26] .

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TlME - Hours 12 , 01' HO 015 '00 , '0 GROUT

OIS'" VOl

/0 -'-'

-.!...LL 10

JO BLEED WATER ... ...

.0 .. q, u '" q, Cl. III

<.) .l...!.. è! "- fil Cl

'" '" ~ ~ 10 5 ,

8 r

_!LL SETTLEO

GROUT

'00

Fig. 5-11 Bleed water (%) for various initial W/C ratios (volume) [26]

The W IC ratio of settled grout (final or effective W le ratio) is smaller

than the initial value at the mixing stage (Fig. 5-12). This is very important

to recognize for the following two reasons:

,- Since the volume of partieles in the mix is decreased because of

bleeding, the overall quality of the grout injected in a crack is

impaired. When the bleeding water evaporates, seeps out or is

absorbed, it leaves the crack partly filled. Thus, the grout stability

is represented by the quantlty of cement particles remaining in

suspension in the grolJt (at rest) sorne time after mixing. A grout is

defined as "stable" when the excess water at the surface (bleed)

of a graded 1000-mL cylinder is less than 5% of the total volume

of the mix, 2 hours after the materials have been mixed (10, 32].

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It is defined as "unstable" if the water at the surface exceeds 5% of the total volume.

2- It is important for comparison of the mechanical characteristics

(compressive strength, modulus of elasticity, etc.) to determine

the final W/C ratio (or true W/C ratio after bleeding). It would be

iIIogical to compare a MC characterized by very little bleeding

with the Type 10 reference cement whose final W IC ratios are

much smaller than the initial values, especially when the initial

W/C ratios are high. Thus, at high initial W/C ratios, the

compressive strength of a Type 10 cement could be greater that

for a MC since its true W IC ratio is in fact smaller.

085 , BY VOL

, ,

'5 ,

)( ~ .....

~ ...., ~ fo-.

J 1 .....

- ~ .....

5 1

8 ,

'1 ,

o 05 1 77

l

\

!\

o 05 7 17

15 7 WC OF ,

~ ~

75 7

SETTLED CEMENT

Fig. 5-12 Example of effective W IC ratios (settled grouts) (26)

55

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To calculate an appraximate value for the effective W IC ratio, the final

coefficient of the volume in suspension, Csf, is multiplied by the initial W/C

ratio, as follows:

Effective W/C = Csf x initial W/C

and Csf = [(Vo - AVf) / Vo] x 100

where Csf = coefficient of the final volume in suspension (%)

Vo = initial volume (ml)

AVf = final bleeding water (ml)

The effective/final W IC ratios are determined by this method in

Section 7.1.

5.4 Factors affecting rheological properties of grouts

Several factors have an influence on the rheology of cement- and MC­

based graut. Von Berg [33J specified that the two most important factors

that have significant influence on these praperties are the W IC ratio and the

specifie surface (fineness of cement grains). The other factors that have a

smaller impact are the cement type (chemical composition), the cement

hydration (time dependency), the temperature, the presence of admixtures,

the mixing time, the mixing intensity.

Most of the effects of these factors were enumerated in the previous

sections but a short summary for each of them is given below.

• Specifie surface

Mehta [23] and Tsivilis [19J have both reported that a finer cement

will have more particles hydrating and shows an increase in the

viscosity of the grout .

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• W/C ratio

An increase in the W IC ratio will decrease the viscos:ty but, at the

same time, increase the bleeding rate and the setting time of the

grouts [3, 4, 8].

• Admixtures (especiallv chemicals)

Superplasticizers will decrease the amount of water needed and will

also decrease the viscosity the grout [10, 15, 23, 26].

• Cement chemical composition

Since the rheological properties are affected when the grout is still at

the fresh state, the most important compound to control is C3A as it

is the tirst one to react with water (and form ettringite needles). It

was seen earlier that gypsum is added to the Portland cement to slow

down the reaction between C3A and water (Mehta (23J calls it

"mechanism ot retardation of C3A by gypsum").

Each cement has its optimum amount of gypsum added to ensure

acceptable final strength and avoid the false set (too much gypsum in

cement and low reactivity of C3A present) and the flash set (not

enough gypsum in cement) phenomena [23].

• Temperatures

The most known effect of the variation of temperatllre on the grout is

the increase of setting time wlth a decrease of temperatures. A low

temperature will slow down the hydration reac1ion between the

cement particles and the water, therefore increaslng the time the

grout takes to harden [16, 23].

57

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• Mixing time and intensity

Houlsby [4J specified that a good mixing will reduce the settlement

and sedimentation (bleedingl problems of a grout. A weil mixed grout

will also have more particles hydrating and improve the penetration in

fine cracks. However, Shwartz and Krizek [16J found that mixing time

and intensity do not have a significant effect on bleeding rate. They

found that only the viscosity is slightly changed (increased) when the grout is weil mixed .

58

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CHAPTER 6

EXPERIMENTAL PROGRAM

This Chapter presents details of the different materials used, the

different tests and procedures followed in this pro,ject.

6.1 Materials used

A total of ten cements were selected for the study: seven microfine

cements from four European and Japanese manu1acturers and two ordinary

Portland cements as references. A Type 10 cement with silica fume was

also tested to verify the effects of mixing time and speed on the rheology of

grouts. Table 6-1 lists the different cements used ln this project (In

descending order of the grain size) and their respe:ctive manufacturer.

Table 6-1 Cements used

Cements Manufacturer

Type 10 Lafarge Cement, Canada Type 30 Lafarge Cement. Canada Type 10SF* Lafarge Cement. Canada Microcem 650 SR Blue Clrcle Co, England Microcem 900 Blue Clrcle Co, England Lanko 737 Lafarge Cement, France SJ!inor A16 Ongny Cement, France MC 500 Onada Cement, Japan 1 Spinor A 12 Origny Cement, France Spinor E12 Origny Cement, France * used for the shnnkage/expanslon tests and

mixing time and speed tests only

Mean gram slze (pm)

16.0 12.0

---

75 5 5 4.6 4.0 3.7 3.5 3.0

1 distnbuted by Geochemical Corp. In North America

Superplasticizers were tested on both the ordinary Type 10 and MCs

(MC500 and Spinors A 12, A 16 and E12). Two different anti-washout agents

were tested on Type 10 Portland ~ement to verify its effects on the grout

rheology.

59

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6.1.1 Cements

The cements used in this study are hydraulic cements that are either

Portland cement or blended Portland cement with blast-furnace slag or other

hydraulic minerai admixture. The other parameter which differentiate these

cements is their grain size analysis as seen in Table 4-1 (coarse,

intermediate or microfine).

6.1.1 Chemical composition

The main difference between an ordinary Portland cement and a MC

is that the former have a much smaller grains size [18]. Both these cements

(ordinary Portland and MC) can be 100% based-Portland or be classified as

blended Portland (see Table 6-2).

A composite hydraulic cement (blended-Portland) is the result of

mixing Portland cement with a pozzolan, or a granulated blast-furnace slag,

or fly ash (see section 4.2.1.4) [22] .

Table 6-2 Cement types

Cement types

Cement 100% 8lended-Portland Portland

Type 10 yes Type 30 yes Type 10SF silica fume Microcem 650SR yes Microcem 900 yes Lanko 737 * Spjnor A 16 slag MC500 slall Spinor A 12 slag Spinor E12 yes * hydraulic ad mixture unknown

60

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The chemical compound proportions (% by weight) presented in

Tables 6-3 and 6-4 were obtained from manufacturers' technical data

sheets.

Table 6-3 Chemical composition (% weight) of cements

Cements Compound Type Type 650SR 900 Lanka Splnar MC Spmor Spmor

10 30 737 A16 500 A12 E12 loss on ignition 2.10 1.50 • • • 1.20 • 1.20 1 20 Insolubles 0.60 0.20 • • • 0.30 • 0.30 0.30 NaO, equivalent 0.87 0.88 0.41 060 • 0.69 • 069 • CaO (free) 0.60 0.90 • • • 1.00 • 1 00 1.00 SiO, 21.20 20.10 19.90 20.2 • 30.50 3060 30.80 22.40 AI,O, 4.30 4.80 3.60 5.50 • 9.60 12.40 10.20 4.20 Fe~O.1 3.10 2.40 520 220 • 1.50 1.10 1.50 490 CaO total 62.80 62.60 64.50 65.30 • 45.8 48.40 4570 6300 -MgO 2.50 2.50 2.00 0.90 • 660 5.80 6.40 • SO~ 320 4.20 330 3.10 • 200 080 320 1 90 TiO, 0.22 0.18 • • • 0.50 • 0.50

P.29~ 023 0.14 • • • 000 • 000 025 SrO • 0.44 • • • • • Na,O 0.32 0.33 0.18 0.23 • 050 • a 50 • Mn,O,\ • 005 • • • • • MnO • • • • • 0.20 • 020 • K,O 0.83 0.56 035 057 • 0.30 • 030 •

TOTAL 97.87 98.30 99.03 98.00 • 91.50 99.10 99.3 96.65

• Data not available

Table 6-4 Bogue composition (% weight) of cements

Cements Compound Type Type 650SR 900 Lanka Splnor MC Spmor Splnor

10 30 737 A16 500 A12 E12 C~S 52.8 55.0 67.0 58.0 - - - - • C,S 20.8 16.4 70 15.0 - - - - • C_':IA 6.0 86 1.0 11 0 - - - - • C~AF 9.5 7.2 7.0 7.0 - - - •

TOTAL 89.1 81.2 91.0 91.0 - - - - • • Data not available - Bogue equations apply only for Portland cements

Differences in the chemical composition of cements will influence a

grout rheological and mechanical behavior. From the above Tables, the

findings can be summarized as follow:

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• Tricalcium silicate (C3S) is an important compound because it

influences the high early strength of the cement and hydrates rapidly

(higher concentration means faster hydration). The C3S concentration

in Type 10 cement is 52.8% whereas that of Type 30 is 55% [16].

This higher concentration for Type 30 cement induces more heat of

hydration compared with the Type 10 cement. Also, Type 30 cement

has a shorter setting time and its strength develops faster [34].

• Microcem 650SR is the only microfine cement that can resist sulfate

attack, since it has a very low concentration of C3A (tricalcium

aluminate).

• The alkali-aggregate reactions are known to be a major cause of

cracking in concrete. Engineers must therefore be sure that the

cement used in grouts for injection does not conta in too many alkalis

(less than 0.60% of equivalent Na02) even if the grout volume is very

small compared with the concrete bulk of the structure [34]. In the

present case, Type 10 and Type 30 Portland cements, Spinor A 12

and A 16 MCs have an equivalent sodium oxide concentration which is

just over 0.60% (Na20 and K20), whereas other MCs (Microcem

650SR and 900, MC500 and Spinor E12) have lower concentrations

than the recommended value of 0.60%.

• The blended (slag-based) Portland MC (Spinor A 12, A 16 and MC500)

can be distinguished by a low concentration of lime (CaO), about

45%, compared with the ordinary Portland cements (Type 10 and

Type 30).

6. 1.1.2 Grain size analysis

The grain size of the cement is indisputably one of the most important

factors to be considered when planning to in je ct a microcrack. The two

reference cements selected for this study are sometimes incapable of

adequately infiltrating certain types of cracks with the result that, if a crack

has only a very small opening and if the cement used contains coarse

particles, the crack may become blocked before it is fi lied (Fig. 6-1) [4, 5].

62

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a} Bridge forming

~ ' ...... ~ .... ~ .... I. '. -------------

b} Clumps forming

Fig. 6-' Grout penetration stopped by a) plug (bridge) and b) grain clumps [4]

A series of tests was therefore performed with a "sedigraph" which

incorporates an x-ray system for determining the size of the cement particles

(Table 6-5 and Fig. 6-2). The procedure eonsisted of introducing 100 g of

cement into a test tube filled with water. The tube was then shaken

continuously to allow the particles to remain in suspension in the liquid. The

grain size was then determined by the x-ray system .

Table 6-6 gives the average (050) and maximum values (0100) of the

cement particles together with their Blaine fineness (the specifie area or

"Blaine" was obtained from the manufacturers' data sheots), The laboratory

measurements were later compared with the values supplied by the

man ufacturers .

63

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Table 6-5 Cement grain size distribution

% passed (weight) Dimension Type Type 650SR 900 Lanko Splnor MC Spmor Spmor

(microns) 10 30 737 A16 500 A12 E12

100 98.3 100.0 100.0 1000 100.0 100.0 100.0 100.0 100.0

70 97.0 99.5 99.5 100.0 100.0 100.0 100.0 100.0 100.0

50 93.0 97.5 99.0 100.0 100.0 100.0 100.0 100.0 100.0

40 87.0 94.0 98.5 100.0 100.0 100.0 100.0 100.0 100.0

35 81.5 91.0 98.0 100.0 100.0 100.0 100.0 100.0 100.0

30 75.5 86.5 970 99.0 100.0 100.0 100.0 100.0 100.0

25 67.5 80.0 95.5 98.0 100.0 100.0 100.0 100.0 100.0

20 585 72.5 91.5 95.0 99.0 100.0 100.0 99.5 99.5

15 48.5 62.0 81.0 895 960 98.0 99.5 98.5 98.5

10 365 43.0 62.0 75.5 865 91.5 97.0 93.0 93.5

8 30.5 41.5 51.5 65.5 76.5 83.5 93.0 87.0 885

6 23.5 33.5 40.0 52.5 62.5 70.5 80.0 75.5 79.0

4 16.5 23.5 26.5 37.5 43.0 50.5 53.5 56.5 63.0

2 70 10.5 10.5 165 14.5 22.0 21.0 25.0 34.0

1 1.5 2.0 1.5 3.5 1.0 4.5 4.5 6.5 8.5

Table 6-6 Cements' mean and maximum grain size and specifie area

Cements Mean Size Maximal size Blaine 050 0100 fineness

(microns) (microns) (m2/kg) Obtained ManullCtur.r Obtalned Manufacturer ManuflCturer

T"ype 10 16.0 18.0 > 100.0 150.0 371

Type 30 12.0 12.0 100.0 90.0 515

Microcem 650 SR 7.5 6.0 70.0 30.0 650

Microcem 900 5.5 4.0 33.0 20.0 915

Lanko 737 4.6 • 23.0 . 700

Spinor A16 4.0 4.5 17.0 16.0 700

Me500 3.7 4.0 170 12.0 900

Spinor A12 3.5 3.5 20.0 12.0 800

S..J!inor E12 3.0 3.5 20.0 12.0 •

• Data not available

The determination of the secondary classification (grain size) of the

hydraulic cements used in the project is possible with Table 6-6. Using the

values obtained in laboratory, the coarse cements are Type 10 and Type 30,

the intermediate are Microcem 650SR and 900, and the microfine are lanko

737 (values rounded down), Spinor A 16-A 12-E12 and MC500.

64

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0\ lA

.......... ?ft -"-Cl) c: li: -c: ~ "-Q)

CL

• • 100 , , , , ,

90 1 1 1 1 1 -.pp,' 0"" I,E b'li ' , , ',1

80 1 1 1 ~~ I,e ~ 1 JI! 1.,.. 1 Il Type 10

:~ 1 1 1 Efm1JINI 1 I~ . 50 1 I,f ,~ A,4 1,. 1 Il' -' 1 1 1 Il ;

Sponor 1112

40 1 1 / H"" A' 1 il I>~ 1 1,< Il ~ SPlnu; ~16

30 1 >'I,Y' h' I><j.q L*1 1 1 1 1 Il ~ SPlnor E12

20 1 ,'>9f+/' -*"T,Je='T 1 1 1 1 1 1 1 Il -Â-

1°~1111I1I1 1 1 III; ~nko737

o 1 10 100

Particle size (microns)

Fig. 6·2 Particle size distribution for different cements

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A close exarnination of the previous Tables and Figure reveals that:

• Type 10 cement grains have a mean size (050) of 16 microns

whereas Type 30 grains have a 050 value equal to 12 microns.

Also, the Blaine fineness (surface area) of cement Type 30 is

about 30% greater than that for Type 10 cement, confirming

results of the particle size analysis.

• The fineness of Type 30 cement is one of the main reasons

why it attains its strength more rapidly than the Type 10

cement. Also, the fineness affects the compressive strength of

the hardened grout: Type 30 specimens are stronger than Type

10 specimens (see Section 5.3.2). However, from the

rheolo!~ical point of view, a finer cement (e.g. Type 30, MCs)

reduces the setting time, may create unwanted volume changes

and inc;reases the viscosity of the grout [19].

• The mean grain size 1050) of ail the other cements varies

betwefm 3 Jlm and 8 J,.lm, which gives a mean size between two

and five times smaller than that for normal Portland cements .

• With a mean grain size (050) of 3 j.tm, Spinor E-12 is the

microfine cement with the smallest grains.

• The maximum grain size of Type 10 and Type 30 Portland

cement is larger than 100 J..lm. Microcracks would therefore be

difficult to inject with normal cement-based grouts and these

cracks should be injected using microfine cements to ensure

that no bridges form inside the microcrack before it is

comph~tely fi lied [4, 15}.

• 050 values obtained with the sedigraph are similar to those

given in the manufacturers' technical data sheets, but the

maximum 0100 values obtained are generally higher than the

manufacturers' values.

• The granulometric curves for the different Mes are similar,

which indicates that the grain distribution within the cement

powder is quite similar for ail of the MCs .

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6.1.2 Superplasticizers

Two superplasticizers were tested with Type 10 cement and Spinor

A 12, A 16 and E12 Mes. One of these SP was melamine-based and the

other one was naphthalene-based (see Table 6-7). Onada and Lafarge

provide their own SPs (with their cement) either in the liquid form (NS200)

or in the powder form in the cement (Lanko 737).

Table 6-7 Superplasticizers used

SP Manufacturer

NS200 Onada

Lanko 737 SP * Lafarge

Eucon Euclid Inc.

Melment Euclid Inc.

• already mixed wlth cement powder

- unknown

6.1.2 Anti-washout agents

Type

-

-Naphtalene

Melamine

Two anti-washout agents (AWA) were tested with Type 10 cement

only ta verify their effect on the rheological properties of a cement-based

grout. One of the AWA was in a liquid form (SC100 fram Sika) and the

other one was in a powder form (Welan Gum distributed by Ciment St­

Laurent).

6.2 Grout and specimen preparation

The decision ta subject the cements (Type 10SF was tested only for

mixing effects and shrinkage tests) ta 13 tests with 8 W/C ratios meant that

over 3000 measurements and specimens (cylinders, cubes, bars) were

needed to study the different rheological and mechanical characteristics

involved .

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For a rational comparison of the characteristics of the different

cements tested, the same specimen preparation method was adopted for ail

cements. Prior to mixing, the cement and ad mixtures (if used) were left at a

mean temperature of 20°C, whereas the initial water temperature was 15°C.

It was decided not to store the materials (cements, water, admixtures) at the

tempe rature of the climatic chambers so that the field conditions could be

better simulated.

Thus, the temperature which is used in the different graphs and

Figures is in fact the curing temperature of the chamber (4°C, 1 QOC and

20°C).

The grouts were mixed at the ambient tempe rature of the laboratory

(about 20°C). Each grout was mixed for 4 minutes at an angular speed of

2300 RPM. About 5.5 l of grout was needed to perform ail the tests for

each W/C ratio. Table 6-8 gives the weight of the cement and water used

for each test, while Table 6-9 gives the number of specimens and the

measurements required .

It should be noted that throughout this study the W/C ratios are

calculated by weight. If a W IC ratio is calculated by volume, it is pointed out

specifically in the text.

Immediately after mixing, the graut bleeding (stability), viscosity and

setting time characteristics (the rheological properties) were tested in the

climatic chamber at the desired temperatures, i.e. 4°C, 1 QOC and 20°C.

Lastly, the cylindrical, cubic and bar specimens (used for the mechanical

tests) were taken and stored in the same chamber. Ali specimens (except for

sorne bars, see Section 6.4.5) were immersed in water for a 28-day curing

period .

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Table 6-8 Weight of Cf3ment and water vs. initial W/C ratio to obtain 5.5 L of grout

W/C Cement Water ratio weight welght

(initial) (kg) (kg)

2.0 2.5 5.0 1.5 3.0 4.5 1.2 3.5 4.2 1.0 4.0 4.0 0.8 5.0 4.0 0.6 6.0 3.6 0.5 7.0 3.5 0.4 7.5 3.0

Onada (MC500) specifies that 1 % of its superplasticizer (NS200)

should be added by weight of cement. Accordingly, the three Spinor

cements (A 12, A 16, E12) were tested with 1.2% (dry weight) melamine­

based superplasticizer added by weight of cement. In addition, extra

rheological tests were performed on Spinor A 12 with the same

superplasticizer but increasing its proportion (by weight) to 4%. Lastly, a

naphthalene-based superplasticizer was tested with different proportions on

Type 10 cement.

It can be seen from Table 6-9 that a minimum of 720 rheologlcal

measurements, 2440 cylinders 5.1x10.2 cm, 240 cubes, 120 saw-cut

concrete-based cylinders and 32 bars were needed for performing ail of the

tests. The effects of the admixtures (superplasticizers and antl-washout

agents) as weil as the mixing rate and time required for the other tests on

the grouts, are in addition to those listed in Table 6-9.

ln the case of the mixing rate and time, only the three rheological

tests were performed on three types of cement wlth three W IC ratios, five

mixing rates and durations, and one temperature (20°C). This added

approximately another 135 or so measurements to the total specified above.

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-.J <:>

• • Table 6-9 Characteristics tested at 40C, 100C and 200C

Charllcteristic No. of No. of No. of No. of No. of No. of No. of No. of W/C Cement Tempera- measurement. cylind •• cube. bars • aw-cut ratio type tur. par W/C 5.1x10.2cm 5.1x5.1x5.1cm 2.5x2.5x cylind ••

par W/C par W/C 25.5cm 7.5x15.0 cm per W/C pet W/C

VISCOSlty 8 10 3 1

Settmg tlme 8 10 3 1

Bleedmg 8 10 3 1 (Stablhty)

Elastlc 8 10 3 2 constants lE. u)

Compressive 8 10 3 3 1 strength Tenslle 8 10 2 2 strength 4 & 20°(';

Bond 2 10 2 3-strength 4 & 20°C

Shnnkagel 1 8 2 2

eXj)élnSlon 4 & 200 e Pulse veloclty 8 10 3 1

Permeablhty and 8 10 3 1 chem. analysis

Microscope 8 10 3 1 analysls (SEM)

8 10 3 3 TOTAL 8 10 2 or 3 10

8 10 3 1 2 10 2 3-1 8 2 2

---- -

• 50 g grout placed between two hOrlzontally saw-cut concrete -based specimens (35 MPa) of 7.5 cm x 15.0 cm

• Tot" No.

of rnusurement • or

specimens

240 msrmts

240 msrmts 1

240 msrmts

480 cyhnders

720 cyhnders 240 cubes 360 cyhnders

120 saw-cut cyhnders

32 bars

240 cyhnders

240 cyhnders

240 cyhnders

720 me.surement. 2240 cyhnders 240 cubes 120 saw-cut cyl. 32 bars

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6.3 Rheologieal tests

This section presents the tests, the procedures a.nd the standards

followed to verify the fresh state properties of grouts. The three properties

that were tested were the viscosity, the bleeding rate (stability) and the

setting time.

6.3.1 Viscosity

Two principal tests were used to verify the viscosity of grouts: the

flow co ne method and the viscometer method. The second approach was

used in this study.

The procedure adopted for the viscosity tests followed the ASTM

Standard 04016-81. A Brookfield viscometer (Photo 6-1) was used to record

the viscosity readings every 15 minutes on 1 aOO-ml grout taken

immediately after mixing .

The advantage of such a method using a digital lV DV 2 + Brookfield

viscometer (l V stands for low Viscosity) is its precision for low viscosities

of about 200 centipoises (cps), yet it gives acceptable values up to 500 cps.

Values exceeding 750 cps are not recorded because the margin of errar

would be too high caused by the Bingham/thlxatroplc behaviors (see section

5.1 and 5.2); theyare simply recorded as being greater than 750 cps.

ln this study, the viscosity values of the various grouts were relative

ta a reference grout and not to water (absolute viscositv of water = 1 cps):

a Type 10 cement-based graut with a W/C ratio (by weight) of 0.6 at the

ambient temperature serves as reference. The value assigned to this

reference grout is set arbitrary ta be 100 cps. Thus, four graphs were drawn

(one per spindle) for this reference grout with different rotational speeds ta

obtain calibration curves (relative viscosity vs. absolute viscosity) for the

cement and are presented in Appendix A.

As it was mentioned above, problems were €:ncountered in this test

because the cement grout does not have a Newtonian behavior, although its

71

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behavior do es become more Newtonian at higher W le ratios or if it contains

a superplasticizer with a high W le ratio. The viscometer is designed for

Newtonian fluids and is much less precise for Bingham fluids such as a grout

especially when it is very viscous (the margin of error increases). The

viscosity readings of a Bingham fluid on the viscometer are "apparent"

values and are not constant for each rotational speed (change the shear

rate) and each spindle used by the measuring device .

Photo 6-1 Brookfield viscometer

6.3.2 Bleeding (stability)

Bleeding is a very important characteristic which indicates how the

grout reacts when left undisturbed for a certain period of time (as in a

crack).

72

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This test was performed in accordance with ASTM Standard C940-89,

"Standard Test Method for Expansion :and Bleeding of Freshly Mixed

Grouts,". The freshly made grout was poured into a graded 1000-mL

cylinder (Photo 5-2) immediately after mixing and the amount of excess

water was recorded at every 1 5 minutes for the first hour, then at every 60

minutes until the two successive readings show no more bleeding (final bleed).

The bleed water reading two hours after mlxlng Îs very important to

define whether if the grout is stable or unstable (see section 5.3). The final

bleed water rate is also important to be known in order to determine the

effective W IC ratios of the grout .

Photo 6-2 Bleeding test

73

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8ecause the bleeding rates recorded are generally low, the different

graphs show the % of volume of cement particles in suspension in the mix

(opposite of bleeding). Thus, the suspension volume (Csf) can Lle computed

as described in section 5.3.

It should be noted that the bleeding (stability) test represents a

vertical crack, since it is performed in a cylinder (see Fig. 6-3). The type of

crack found in the structure should influence the container used for this test:

for example, if the crack is horizontal, the test should be performed on a fiat

horizontal bucket.

Crack type Model used

Horizontal crack Flat bucket

4--~

Vertical crack Vertical c linder

Fig. 6-3 Crack types and suggested model for bleeding test

6.3.3 Setting time

The setting time is the last rheological characteristic ta be verified.

The time that a freshly mixed grout takes to set is basic information which is

needed before injection takes place. Rapid setting must be prevented or else

it will black (plug) the crack opening or the pipes of the injection equipment.

On the other hand, tao long a setting time or fallure to s,~t is harmful

because the grout may be washed out by the flow of water or freeze if the

temperature drops below QOC.

74

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.... -------------------_ .....

The setting time is defined as the time taken by a cement grout to

harden [20] and it depends mainly on the cement grain hydration rate, which

is governed by the amount and crystalline form of C3A and C3S. The

hydration rate is influenced by the various factors including the tempe rature,

chernical composition, cement particle size, W/C ratio and the presence of

admixtures. Considering the lower and the upper limits of the W le ratio

(0.4 to 2.0), this time may vary between 15 minutes to values more than 24

hours, depending on the factors mentioned above.

The ASTM Standard C191-82, "Standard Test Method for Time of

Setting of Hydraulic Cement by Vicat Needle, n describes the test procedure

used. A small amount of grout (-120 ml) is placed in a standard co ne­

shaped mold immediately after mixing. Readings are taken at regular

intervals with the Vicat apparatus (see Photo 6-3) ta obtain the initial and

final setting times .

Photo 6-3 Vicat apparatus

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._--

The initial setting time is recorded when the needle penetrates 25 mm

or less into the sp(-3cimen, while the final setting time is the time the sample

takes to set cornpletely, which is recorded when the needle no longer

penetrates into the hardened specimen.

6.4 Mechanical tests

The main reasons for injecting grouts into cracks in hydraulic

structures are to consolidate it, to stop water infiltration (watertight) or just

to fill (seal) the voids. The mechanical ch=uacteristics of the hardened grout

have a decisive effect on the selection of a suitable product which must be

compatible with the base concrete to avoid debonding due to tensile or

shear stresses inside the crack [351.

This section describes the tests performed on hardened grout at three

temperatures. The specimens were Bil prepared and immersed in water for

28 days in a climatic test chamber at the required temperature to cure. The

following mechanical tests were conducted:

• Modulus of elasticity and Poisson's ratio.

• Compressive strength.

• Indirect tensile (splitting) strength.

• Bond strength (tensile).

• Shrinkage/expansion.

• Ultrasonic pulse velocity.

• Water permeability and leached water analysis.

• Microstructural characteristics.

6.4.1 Modulus of elasticity and Poisson's ratio

The values of the modulus of elasticity (E) and the Poisson's ratio (u)

provide an indication of the stress that the hardened graut can resist

elastically (in the case of cement or concrete, it not perfectly elastic) and the

acceptable amount of deformation in this elastic zone .

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----------------------

The modulus of elasticity is the ratio (slope) between the axial stress

and the st.rain (bath in the longitudinal direction) during a uniaxial

compression test, which provides information about the stiffness of the

material.

A combined compressometer-extensometer system, attached ta the

cylindrical specimen (5.1 cm x 10.2 cm) which was then loaded by a

hydraulic compression machine (see Photo 6-4), was used ta determine the

values of E and u. The ASTM Standard 03148-86, "Standard Test Method

For Elastic Moduli of Intact Rock Core Specimens in Uniaxial Compression,"

was followed for this test .

Photo 6-4 Hydraulic compression machine

77

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The values for E were obtained by calculatrng the slope of the aXial

stress versus the axial strain whereas the values for l> are calculated from

the results for the modulus of elastlcity as follows:

E = slope of 3xial curve at 50% of ultlmate

strength (crult)

= (cra2 - C'a1) / (ca2 - ca 1)

and u = (-E)/(slope of the lateral curve)

where: E = Tangent modulus of elasticity (Pal

u = Poisson's ratio

cra = Axial stress (Pa)

ca -- Axial strain

6.4.2 Compressive strength

Il- graut in the hardened state which has a poor compressive strength

should not be considered as a good consolidation product for a structure

that has a cracking problem. The loads applied, stresses or displacements

could damage parts of the structure that have been strengthened with a

poor-quality grout. It is, therefore, important to idEntify the different factors

that affect the grout strength.

The compressive strength (fc ') is the maximum axial force that the

arOIJt specimen can withstand. Cylindncal (5.1 x 10.2 cm) and cube­

shaped (5.1 x 5.1 x 5.1 cm) specimens were used. After unmolding, ail of

the specimens were immersed in water for 28 days, whereupon a rydraullc

machine was used to determine the compressive strength using the ASTM

Standard C942-86, "Standard Test Method for Compressive Strength of

Grouts." for the cubes and the ASTM Standard D2938-86 "Unconfined

Compressive Strength of Intact Rock Core Specimens" for the cyllnders.

6.4.3 Indirect tensile (splitting~ strength

This test pravides an indication of the tensile stresses that the graut

can withstand (i.e. in a filled crack).

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ln order to reduce the amount of different type~ of specimen

prepared, the indirect method was preferred to the direct tensile strength

test (where "bone" specimens must be prepared). This is why the so-called

Brazilian or indirect or splitting Illethod based on tt.e ASTM Standard 03967-

86, "Standard Test Method for Splitting Tensile Strength of Intact Rock Core

Specimens" was used; the latter is performed on Jlhe cylindrica! hardened

grout specimens which are saw cut to 2.5 cm long. Thase 2.5-cm disk are

placed vertlcally betwüen L ') perfectly parallel steel surfaces and a

hydraulic machine applies a load whi:;h increases constantly until the

specimen splits in two

6.4.4 Bond strength

Once the grout has set in the crack, it must bond complately with the

surrounding base concrete to effectively strengthen the structure. Cement­

based grouts should have a particularly strong bond strength with concrete

because they are both slmilar. It is, therefore, expected that since the two

materials have similar thermal expansion coefficients, they undergo similar

the~mal deformations wh,ch eliminates any new cracking problems.

The bond strength may be defined as the m~ximum axial tensile

strength that the hardened grout has to withstand when the surrounding

base concrete shifts and tries to re-open the grout-filled crack. To obtain

values for this factor, more complex specimens had to be prepared. A small

amount (50 g) of fresh grout was placed between two concrete surfaces (a

concrete cylmder (35 MPa) 7.5 x 15 cm sawcut in ha If) repre:;enting the

crack on a small scale.

After 28 days of curing in a moist chamber, they were tested with a

direct tension machine (Photo 6-5). The standard followed in this test is an

in-house procedure developed at IRED's concrete laboratory.

The initial W/C ratios used were the lower W/C ratio limits, Le. two

initial W IC ratios (usually 0.4 and 0.5) with the highest viscosity values, of

each cement studied.

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Photo 6-5 Tensile strength machine

6.4.5 Shrinkage/expansion

After a cement-based grout has been injected in a crack to strengthen

the structure, bleeding may appear and proceed at different rates until the

graut sets. Even after the grout has hardened uver a period of several days

or possibly years, the cement particles continue to hydrate if moisture IS

present in the crack. Throughout that time, the hardened grout may elther

shrink or expand, depending on the characteristics of the cement (chemical

composition) and the ambient t:umidity.

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Shnnkage or expansion of hardened grout can cause serious

problems. If shrinkage occurs for Jack of moisture, the crack may reopen,

reducing the water tightness of the structure. If, on tha other hand, the

grout expands with the ~><cess rnoisture pr&sent the concrete may be

exposed to qUlte signiflcant stresses, especially if the crack is large.

The first step in this test is to make standard bars of the des1red grout

(initial W IC ratIo of 0.6) in !engths of 254 mm with a section area of 25.4

mm x 25.4 mm. Linear length change readings are then taken (,'lce a day for

the first seven days and opr.e a week after that for the remaining three

weeks. Sorne bars are placed in a moist environment and others in a dry

one. This tes~ was also performed at two different curing temperatures: 4°C

and 20°. The ASTM Standard C531-85 ("Standard Test Method for Linear

Shrinkage and Coefficient of Thermal Expansion of Chemical-Resistant

Mortars, Grouts and Monolithic Surfacings") is the stanoard followed.

6.4.6 Ultrasonic pulse velocity

The ultrasonic pulse velocity test is a nondestructive means of

obtaining data on some of the elastic characteristics (Ed, vd) of a cement­

based grout. This technique is used to determine the hardened graut

uniforrlity. Uniformity of the graut leads to faster velocities and usuall'{

better an improved strength [36].

The ultrasonic. pulse velocity is defined as the propagation speed of

the longitudinal and transversal waves of a pulse signal through a solid. The

two velocities obtained are ther. used to ca!culate a dynamic elastic

constants (modulus of elasticity and Poisson's ratio) of the graut [37].

The procedure to complete this test is fairly simple. A transducer

emits an ultrasonic pulse thraugh the grout specimen and this pulse is

received on the other side of the specimen by another transducer (see Fig.

6-4). The time taken by both pulses to travel through is recorded élnd the

length of specimel1 was also recorded prior to the test. Then, the pulse

velocities are computed wlth both the time of travel and the length traveled.

81

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The ASTM Standard D2854-83, "Standard Test Method for

Laboratory Deter.nination of Pulse Velocities and Ultrasonic Elastic

Constants of Rock" 1 was followed for this test.

Pulse Generarar Un.1

r"9ger mo.n oulpul 00ulpul

ï -....., 1 Preomplof •• , 1

l ___ J

r - - 1 f'8ec-;;';I't- -l Osclllo,cope

IT.me Delay 1 1 Ûlunler ~ CIrCUI'

L ..2...l 'lorI ~toP..;-I_--'_.oi--T~ _______ - __ ~ _____ ~ ___ ~-~

Fig. 6-4 Schematic diagram of ultrasonic apparatus [36J

The important factors that affect the ultrasonic pulse velocities (2) are

the mineralogical characteristics, chemical composition, porasity and the

moisture content of the cement-based graut.

The values of the dynamic modulus of elasticity (Ed) and the Poisson's

ratio (vd) are derived tram the longitudinal (a Iso called "compression") and

transversal (also ca lied ushear U) wave velocities, computed using the

following formulas [37]:

82

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where Ed = dynamic Modulus of elasticity (GPa)

vd = dynamic Poisson coefficient

p = density (kg/m3)

Vs = transversal (shear) velocity (mIs)

Vp = longltudl.lal (compression) velocity (mIs)

These dynamic propenies (Ed and vd) must not be confused with the

"static" praperties described in Section 6.4.1. They are obtained fram

different tests, the first series being destructive (E and v), the second being

nondestructlve.

6.4.7 Permeability and leached water analysis

The permeability of a cement-based grout filling a crar:k of a hydraulic

structure affects the durability, service life and other properties of the

material. It is, therefore, important to ensure that the hardened grout will

not be extremely porous or friable in the location (cracks) where it is

intended to remain for many years. The permeability test is consequently

designed to measure the degree to which a glven arnount of water can

penetratG Into and through a hardened cement-based grout.

Permeability may be defined as the ease with which a fluid can flow

through a solid [23].

The factors that influence the perrneability include the W/C ratio

(which affects the size and contrnuity of the pores in the paste), the cement

type, the chemical additives, the applied loads, the temperature variations,

the humidity level, the attilcks by chemicals such as sulfates, Gdds, etc.

ln fact, the amount of mlxing wélter is the main source of permeability

problems of the hydrated cement paste, because It contrais the total space

and the unfilled spa(~ after the water is consumed by the cement hydration

(or evaporation) [23]. Table 6-10 contains permeability values of cement

versus the number of curing days and it can be compared with the

permeability of some known rock~ in Table 6-11.

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Table 6-10 PermeClbilitv of cement paste (W le = 0.7) wi'lh the progress of hydratlon [23)

Age Permeablltty

(days) lcm/sec x 10-11 )

rres~ 20,000,000

5 4,000

6 1,000

8 400

13 50

24 10 .-Ultlmate 6

Table 6-11 Permeability of cement pastes and different rocks [231

Type of rock Permeablhty W le ratio of mature (cm/sec) pûste of the sa me

permeablllty Dense trap 247 x 1O-1 :l 038

Quartz diorite 824 x 10- 1L 0.42 Marble 2.39 x 10- 11 048 Marble 5.77 x lO- IU 0.66 Granite 5.35 x 1O-~ 070

Sands1:One 1 23 x lO-tl 0.71 Granite 1. 5b x 10-tl 0.71

The leached water analysis (chemlcal analysis of the water collected

by the permeability measuring device) serves to determme the chemical

components of the hardened grout that are removed or leached by the water

flow through the specimen.

These two tests are therefore complementary: after the permeability

test, the water (if any) collected 15 used for the chemical analysis test using

a procedure developed at Sherbrooke University [381.

84

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6.4.8 Microstructural characteristics

Cements are distingUished mainly by their chemlcal composition and

grain size. Mlcroscoplc analysis of the hardened grout reveals the impact of

the different chemlcal elements, crystal structures and general appearance

(pOroSlty, roughness, etc.) of the specimens examined.

A scanning electron microsccpe (SEM) was used to magnify the

specimens to micron size and the dlfferent crystalline forms of the hardened

grout were then analyzed. The SEM permits the observation of massive

crystals of calciurr, hydroxlde, the flbrous morphology of C-S-H crystals

(these are poorly crystalline), tne ettringite crystals (short prismatic needles),

the gypsum need!es in pores jf a taise set occurred, etc [23].

The most significant physical charactenstics to be observed with the

SEM are the po rosit y of the paste, the mternal cracking (microcracks) and

the roughness of the breaking surface .

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CHAPTER 7

EXPERIMENTAL RESUl TS AND DISCUSSION

This chapter presents the results obtamed from the dlfferent tests

performed on the grouts. Detailed analysis (taking mto account the dlfferent

factors that may have an effect) ar~ performed for each rheological and

mechanical characteristics of the MC-based grouts.

The effective (final) W/C ratios is determined to establlsh a fair

comparison tool for the mechanical propertles of the different cements since

each of them has a different bleeding rate.

7.1 Determination of effective W/C ratio

Using the equations given in Section 5.3 and the results of the final

volume in suspension (opposite of final bleeding rate) in Table C-2 (Appendlx

Cl, the computed results are presented in Table 7-1. It can be noted ln

Section 7.3 (effects of temperature) that the variation of temperatures (4 oC,

10°C and 20°C) does not influence the bleedmg rate. Thus, the computed

values of the effective W/C ratios were calculated using the average of the

final volumes in suspension.

Table 7-1 Effective W/C ratios vs. initial W/C ratios

Initial Effective W IC ratio W/C Type Type 650SA 900 Lanka Splnor MC500 Splnor Splnor

ratio 10 30 737 A16 tSP A12 E12

0.4 040 0.40 040 0.40 040 040 040 040 0.40

0.5 049 050 050 050 050 050 050 050 050 --f----r-----0.6 057 059 060 059 059 060 060 060 060

08 064 0.73 079 080 079 080 080 080 o BD

1 0 0.71 085 098 098 091 1 00 098 099 100

1.2 076 o 91 1 13 1. 16 1 01 1 16 1 19 1 19 120 ---'--- ----

1.5 082 1 02 1 20 1 25 1 18 1 36 145 1 :. 7 1 50

2.0 084 i 09 1 23 1 56 1 31 165 1 70 18-6 1 99 ----

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The effective W/C ratio of norrT'al Portland cement grout such as Type

10 and Type 30 is strongly affected bV its bleeding. As an example, the

effective W/C ratio for Type 10 grout varies tram 0.40 to 0.84 compared

with its initial W IC ratio of 0.4 and 2.0, respectiv"3ly. The MC grouts have

effective W IC ratios which are similar with their initial W IC ratios because

the bleeding of water is less important in their case.

7.2 Effeet of W le ratio

This section determines the effect of the variation of water/cement

ratio on the rheological and mechanical properties of MC-based grouts.

For the rheological properties, the initial W IC ratio~ were used

whereas for the mechanical i'roperties the effective W IC ratios were chosen

far the comparison or the properties for the various cements.

7.2.1 Rheologieal characteristics

The three characteristics studied are the viscosity, the volume in

suspension after two hours (to define whether the grout is stable or

unstable) and the setting time.

• Viscosity

As mentioned earlier, the viscosity values are relative to a Type 10

cement-based reference grout with an initial W/C ratio of 0.6.

Tables 8-1 and 8-2 (Appendix B) give the relative viscosity values

obtained just after mixing and 60 min after mixing, respectively, white

Figures 7-1 and 7-2 show the variation of the relative viscosity with the

initial W/C ratios at a temperature of 20°C.

The results of the viscosity test obtained with a Brookfield viscometer

raise the tollowing points:

87

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• The relativ~ viscosity values are inversely proportional to the

initial W IC ratio for ail of the different Portland cements and the

MC-based grouts. Therefore, an increase of the initial W IC ratio

decreases the graut viscosity. The different curves (shown) ln

Figures 7-1 and 7-2 generally follow an exponential law (~I = a

x 1 Ob(W IC)), but each cement has different value for the

constant "a" and "b".

• Type 30 cement-based grout is more viscous than Type 10

grout, especially for low W/C ratios (0.4 and 0.5), possibly

because of its greater fineness and greater concentration of

C3A (accelerates early hydration reaction) (19).

• The finer the cement, the more viscous is the graut. In general,

Type 10 and 30 (coarse cement) have the lowest viscosity

values, followed by the two intermedlate cements (650SR and

900) and closing with the MCs (MC500, A 12, A 16 and E12).

Lanko 737 is less viscous than Type 10 grout although it has a

greater specifie area, but as it was mentioned, a SP agent is

added to its cementious powder by its manufacturer.

• As expected, Spinor A 12, A 16 and E12 cements are less

viscous when mixed with SP. It can be seen that with dlfferent

SP proportions, Spinor A 12 has relative viscosltles decreasing

êlS follows for a W/C ratio of 0.8: 400 cps (no SPI to 6 cps

(1.2% SPI to 3 cps (4.0% SPI. The two blended Portland-slag

MCs (Spinor A 12 and A 16) have relative viscosity values

smaller than the Type 10 grout when they are used with a SP.

The Spinor E12, even with 1.2% of SP, is still more viscous

than Type 10 cement graut, but it is clear that the addition of a

SP with a MC-based graut is essential to have low viscosities

comparable to Type 10 cement graut.

• The viscosities are higher after 60 minutes (as expected) since

the hydration of certain cement compounds (especially C3A)

have started .

88

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• 600 ... 500

Type 10 - 009-fi) Type 30 a. 0 "* - 400 900 ~ ..-ën 650 SR

8 300 • fi) MC 500 +SP '5 il-Q)

200 Lanko 737

> ~ CU 'i\ ct:: 100

o 0.5 1 1.5 2 Initial W/C ratio

• 600 -500 Type 10 - .....

(/) A12 a. 0 "* - 400 A12 + SP(l,2%1 b • 'i;; A 12 + SP(4,O%1

8 300 (/) 'S; Q)

200 > ~ CU Q)

0:: 100

o 0,5 1 1.5 2 Initial W/C ratio

• Fig. 7-' Relative viscosity just after mixing at 200C

89

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600

- 500 VI Q. 0

-Type 10

+-----------------------------~~ A16

* - 400 . ~

~----------"r_------_..I A16 ... SP\1,2%' ... en 8 300 li) .s; Q)

200 > :;:::1 co Q)

0:::: 100

0

E12 .. +-----------..... ~------...." E12+SP(1,2%1

0 0.5 1 1.5 Initial W/C ratio

Fig. 7-' (cont'd) Relative viscosity just after mixing 20°C

600 -500 Type 10 - ..q..

li) Type 30 Co 0 * - 400 900 ~ ... en 650 SR

~ 300 .. MC 500 +SP

'S; ..... Q)

200 l.nko 737

> :;:::1 as Q) ·v 100 L ••

2

l' 1

o -'-+--+-+---+--4-':;'=~~~:;;;:I ~~ E~~ o 0.5 1 1.5 2

Initial W/C ratio

Fig. 7-2 Relative viscosity (at 60 mini at 200e

90

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• 600 -500 Type 10 - ......

ln A12 Co

* 0 - 400 A12 + SP(l,2%1 ~ ... fn A 12 + SP(4,O%1

8 300 ln '> Q)

200 > ~ CU Q) a:: 100

O~~~~~~~~~~~~.-~~.

o 0.5 1 1.5 2 Initial W/C ratio

600 • -Typ, 10

- 500 ...... fi) A16 Co

* 0 - 400 A16 + SP(l,2%1

~ ... 'ii) E12

8 300 • fi) E12 + SP(l,2%1 'S; Q)

200 > ~ CU Q) a:: 100

o 0.5 1 1.5 2 Initial W/C ratio

Fig. 7-2 (cont'd) Relative viscosity (at 60 min) at 200C

• 91

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• Bleeding (stability)

The volume in suspension of cement in a grout (Tables C-l and C-2 in

Appendix C) is one of the properties which, like the viscosity, is sensitive to

slight variations in the initial W/C ratio. The results shown in Figures 7-3

and 7-4 lead to the following conclusions:

• The volume in suspension values are inversely proportional to

the initial W IC ratio for ail of the ordinary Portland- and MC­

based grouts. Therefore, an increase of the initial W IC ratio

decreases the graut suspension volume.

• The suspension volume of normal Portland cements grouts

(Type 10 and Type 30) d~creases rapidly when the initial W IC

ratio is increased. The stability criterion (less than 5% of bleed

water on the surface after 120 minutes) is therefore greatly

affected by a variation in the initial W/C ratio. Type 10 cement

graut is considered unstable from an initial W/C ratios of 0.6

and up whereas Type 30 cement is unstable with an initial W IC

ratios ~ 0.8. The grain fineness of Type 30 cement is the reason

of its slightly better performance.

• The majority of the intermediate (650SR and 900) and MC

grauts are stable even when the initial W IC ratio is high (Iarger

than 1.2). Their fine.less is the main cause of the smaller

bleeding rate. Thus, finer is the cement with a higher W/C ratio

results in a more stable grouts. The finest MC grouts tested in

this st .. dy was Spillor E12, which is stable up to an initial W/C

ratio of 2.0.

• The final suspension volume are almost identical to the on es

recorded after a period of 1 20 minutes when the initial W IC

ratios are lower than 1.0. In the case of both the intermediate

and microfine cements, the differences between the final and

the 120 minutes values are less than 5 % even at the highest

W/C ratios .

92

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100

-~ 80 0 -Q)

E :J 60 0 > c: 0 40 'in c: Q) Co 20 fi) :J en

100

-~ 0 80 -Q)

E :J 60 ~ c:

40 0 en c: Q)

20 Co fi) :J en

0

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

_Type 10

fm1900

0.4 0.5

_Type 10 œ1A16

~Type 30 D650SR ~MC500+SP • Lanko 737

0.6 08 1.0 1.2 1.5 2.0 Initial W/C ratio

~E12 DE12+SP(1,2% ~A 16+SP(1 ,2%)

Fig. 7-3 Suspension volume after 120 min at 20°C

93

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100 -';/. - 80 Q)

E :::::1

g 60

§ 40 "iiS c:: 8. 20 fi) :::::1

(J)

o 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

.Type 10 ~A12

DA12 + SP(1,2%) œ)A12 + SP(4,O%)

Fig. 7-3 (cont'd) Suspension volume after 120 min at 200C

100

-?ft. 80 -Q)

E :::::1 60 (5 > c: 0 40

'ii) c: Q) Co 20 f/J ::J

CI)

0 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio .Type 10 ~Type 30 D650SR .900 ~MC500+SP gLanko 737

Fig. 7-4 Final suspension volume at 20°C

94

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100 -?f. - 80 Q)

E ::::J o >

60

5 40 'u; c: Q) o. 20 '" ::::J en

100

-?f. - 80 Q)

E :::l

g 60

5 40 'u; c: ~ 20 '" :::l en o

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

.Type 10 BA16

~E12 DE12+SP(1,2% ~A 16+SP(1 ,2%)

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

_Type 10 ~A12

DA12 + SP(1,2%) rBA12 + SP(4,O%)

Fig. 7-4 (cont'd) Final suspension volume at 200C

9S

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• Setting time

The setting time is very sensitive to the variations of the initial W IC

ratios as shown in Tables 0-1 and 0-2 (Appendix D) and in Figures 7-5 and

7-6.

• The setting time varier. proportionally with an increase in the

initial W/C ratio for ail cement grouts. Sy adding more water to

the mix, the cement grain concentration decreases (the excess

water slows down the hydration reaction) and it takes more

time for the graut to set and harden.

• Type 10 and Type 30 cement grouts have the longest setting

times of ail cements (without SPs) studied in this project.

• The MC fineness and their chemical composition are the main

factors responsible for their lower setting times than the

reference Type 10 cement. It should be noted that SP should be

used in sorne cases (i.e. Spinor E12 at low W/C ratios) to

increase the setting times to avoid plugging of the microcracks

(especially if the initial W le ratio is low) .

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30r---------------------~~==~ ... 25 +-----------------t ~e 10

Type 30 -M­

~ 20 +------------------i 650SR

~ * o ~ 15 ~ -Q)

~ 10 +-----~~~~-------.,

5 +-----~~~---~.----------------~

0~~~~4_~~~~~~~~~~~~

o 0.5 1 1.5 2 Initial W/C ratio

30 ... 25

Type 10 09-MC500+SP -Mo

- 20 Lanko 737 f!? ... ~ E 12

~ 15 .... - E12+SP(1.2%) Q)

E 10 ~

5

0 0.4 0.5 0.6 0.8 1 1.2 1.5 2

Initial W/C ratio

Fig. 7-5 Initial setting time at 200C

97

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'.

30 ... 25

Type 10 09-A 12

"* - 20 A12+SP(1,2%1 ~ ... ::::s

A 16 0 .c 15 ... '-" Q)

A16 +SP(1,2%1

E 10 i=

5

o 0.5 1 1.5 Initial W/C ratio

Fig. 7-5 (cont'd) Initial setting time at 200C

30

25

- 20 e? ::J 0 .c 15 '-" QJ

E i- 10

5

0

.... Type 10

~----------------------------------------------------------------~~ Type 30

+--------------------------------------------------~~ 650SR

0 0.5 1 Initial W/C ratio

1.5

.. 900

Fig. 7-6 Final setting time at 200C

98

2

2

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• 30 l===-===::;--------------,

Type 10

25 09-MC500+SP

"* ...-. 20 Lanko 737 ~ .... :J E 12 E. 15 .. Cl) E12+SP(1,2%)

E i= 1 0 +----~---:79----------_t

5 +----------+----------------------~

o 0.5 1 1.5 2 Initial W/C ratio

• 30 ... 25

Type 10

~ A 12

"* ...-.20 A12+SP(1,2%) ~ * :J

A1S 0 ..c: 15 .. - A16 +SP(1 ,2%) Cl)

E i= 10

5

0

0 0.5 1 1.5 2 Initial W/C ratio

• Fig. 7-6 (cont'd) Final setting time at 200C

99

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7.2.2 Hardened grout characteristics

Several mechanical characteristics can be verified using the tests

mentioned in Section 6.4. The results of these tests are given below,

keeping in mind that the emphasis is placed on the effects of the variation of

the W/C ratios .

• Modulus of elasticity and Poisson' s ratio

The values of the modulus of elasticity (El and the POlsson's ratio (ul

were obtained (see Tables E-1 and E-2, Appendix El after the 28 day curing

period of the cylindrical specimens.

Analysis of Figures 7-7 and 7-8 uses the initial and effective W/C

ratios, respectively, to show why the effective W/C ratios (only up to 0.85,

because it corresponds to Type 10 highest effective W/C ratio) should be

used when comparing different cement grouts that have different bleedlog

rates. It can be seen in Figure 7-7 that when the initial W IC ratio is low

(very little bleeding for ail cements), the reference Type 10 grout has the

lowest E values, but when the initial W IC ratios increases to 0.8 and hlgher,

its E values are higher than for most of the other cements (intermediate and

microfinel.

Figure 7-8 (using effective W/C ratios) shows that the micro fine

cements (Spinor A 12, A 16, E12 and MC500 + SPI have then higher Evalues

than for the Type 10 cement for ail the ratios. The Idea IS to compare the

mechanical properties of two cement specimens that used the sa me amount

of water to hydrate and the same "true" W/C ratio of settled particles to

establish a fair comparison of the different types of cement.

The main observations concerning the se two parameters follows:

• The modulus of elasticity of the grouts decreases as the W IC

ratio increases (E is inversely proportional to W IC).

100

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20~----------------------~==~ • il10 -cu Q.

~ 15 ~ ·0 ~ CI)

cu 10 1) ..... o

5

o

H-------------------------~Ej~ Il iii

.~m_ ...... --..... -------_; L.nko 137

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

20r--------------------------------~~ -cu Q.

~ 15 ~ '0 1;; -m 10

o CI) ::J :; 5 "0 o ~

o 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

Fig. 7-7 Modulus of elasticity vs. initial W/C ratios at 200 e

101

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20

-cu Q.

~ 15 b '0 ~ rn : 10 't-o rn ::J -::J 5

"0 o ~

a

20

't-o fi)

; 5 "0 o ~

o

.

0.40

0.40

• . . • 0.50 0.60 0.70

Effective W/C ratio

1

L . 0.50 0.60 0.70

Effective W/C ratio

• tIl'O ,~,

tj~ ~

Ëi ---

fil ~ lanko 737

'- 1--

~

0.80 0.90

• fit 0 1-

~ --

~ Il t-E"

• . 0.80 0.90

Fig. 7-8 Modulus of elasticity (GPa) vs. effective W/C at 20°C

102

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• At a temperature of 200 C, the reference cement Type 10 grout

has modulus of elasticity values which vary from 14.3 to 6.1

GPa with effective W/C ratios of 0.40 to 0.85, respectively (a

30 MPa concrete has a Evalue near 28 GPa [23]). The values

for Type 30 cement grout can be seen ta be about 200/0 greater

than for those of Type 10. The greater concentration of C3S

and the fineness of Type 30 cement are the factors responsible.

• Spinor (A 12, A 1 6 and E 12) MC grouts have a higher modulus

of elasticity than for the Type 10 cement grout (at 200 C) up ta

an effective W/C ratio of 0.80, indicating that grain finenes:-,

plays an active raie.

• The Poisson's ratio (v) of the hardened graut specimens varies

between 0.10 and 0.18 close ta the value for normal concrete

For example, a 30 MPa concrete has a v value of 0.15 to O. 18

[23] .

• Compressive strength

The compressive strength (fc') is the maximum axial stress resisted by

the grout cylindrical specimens. The results used here are the ones that

were obtained with the cylinders because their average values were better

than the values obtained with the cubes.

Figures 7-9 and 7-10 show the compressive strength as a function of

the initial and effective W/C ratios (the complete results are present in Table

F-1, Appendix F).

• The compressive strength, fc', is inversejy proportional to the

increase in the W IC ratio for ail the cement grouts.

(~ The effective W/C formulation allows Type 10 cement graut ta

be identified as the weakest cement. This was expected

because this cement has the lowest concentration of C3S and

the coarsest particles [19].

• ln general, Micracem 650SR (highest C3S content) and Lanka

737 MCs are the strongest cements studied in this

investigation.

103

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80

70

60

_50 ca ~ 40 -~ 30

20

10

0

80

70

60

_ 50 cu

~ 40 -~ 30

20

10

0

• _10 P

Ej30 rlf - -

Il Lanka 737

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

• +-________________________ ~~10

~----------<lD ~-----____4~

fil .... --~ ___ __m......._------.--____4 E12

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

fig. 7-9 Compressive strength vs. initial W/C ratio at 20°C

104

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80

70

60

co 50 a. ~ 40 -S 30

20

10

o

80

70

60

(ù 50 a. ~ 40 -S 30

20

10

o

1-

.

• 1 1

0.40 0.50

. 0.40 0.50

• 1-

fit ~30

li iii Lanko 737

• .1 J .1 1 -.-

0.60 0.70 0.80 0.90 Effective W/C ratio

• ~ _'0 0 ~

Ir ~

Il E12

J. --' J .1 1 . . 0.60 0.70 0.80 0.90

Effective W/C ratio

Fig. 7-10 Compressive strength vs. effective W/C ratio at 200C

105

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• The fc' values ~btained for the blended Portland-slag cement

grouts (Spinor A 12 and A 16, MC500), tested after 28 days at a

curing temperature of 200 e are slightly higher than those of the

reference Type 10 cement grouts.

• Bond strength

Most of the time, the hardened grout failed in a crack because of its

poor bond strength.

ln spite of low values obtained (see Fig. 7-11 and Table G-1 in

Appendb" G), the following observations can be made:

• As for the compressive strength and the modulus of elasticity,

the tensile bond strength is inversely proportional to an increase

of the W/C ratio .

• With the low values obtained for ail cements, it is difficult to

analyze the bar charts but it shows that the microfine cements

have a better bond resistance to tensile forces than ordinary

Portland cement grout.

• Type 10 has the lowest tensile bond strength, approximately

0.2 MPa, at both effective W/C ratios of 0.4 and 0.5

106

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2.0----------------------------------1.8 .J--------------jr. • ..-----" 1 6 Type 10 m . +-------------.---------------~[]

a.. 1.4 Type 30 ~ ~ ';; 1.2 650SR ~ ~ ~ 1.0 900

~ 0.8 ~ 'u; Lanko 737 ij 0.6 +---=

1- 0.4

0.2 0.0

0.4 0.5 0.6 0.8 1.0 Effective W/C ratio

2.0...------------r===:::::;, • 1.8 +---------------4 Type 10

1.6 0 m M6 a. 1.4 ~ ~ MC500+SP i 1.2 lm ~ 1.0 ; ~ 0.8 E12 'u; '----... ij 0.6 +------1- 0.4 i-----;"1ê§

0.2

0.0 0.4 0.5 0.6 0.8

Effective W/C ratio

Fig. 7-11 Bond tensile strength at 200C

107

1.0

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• Shrinkage/expansion

The bars (made with an initial W/C ratio of 0.6) were tested in two

different environments: the first is a very humid one (100% relative

humidity) and the second is dryer environment (Iess than 30% relativo

humidity). Thus, the shrinkage and the expansion were more easily

perceptible on a shorter period of time.

The results are presented in Figures. 7-12 and 7-13 where shrinkage

values are considered as negative and expansion values as positive. As

expected, bars cured in water expanded whereas those left in a dry

environment shrank.

• The Type 10 cement-based grout expands when submerged in

water (humidity = 100%) and shrinks when left in a dry

environment (humidity less than 30%). However, the shrinkage

phenomenon was more important than the expansion one. Thi0

confirms that hardened cement paste needs water fer a certain

time to complete its hydration (not only in the first hours after

mixing). Another reason which also ex plains shrinkage in a dry

environment is the effect of capillary water; when the water

molecules held by capiilary tension in small capillarles (5 to 50

nm) is removed (evaporation) in a not-so humid environment, it

may cause shrinkage of the specimen [23].

• Type 30 cement grout expands twice as much as the Type 10

cement grout, and it also shrinks more than Type 10 when the

specimens are located ill a dry environ ment. The chemical

composition is the main factor which contributes to this

difference in the behavior of the two grouts.

• Type 10SF (8 % silica fume added by the manufacturer) did not

expand as much as for ordinary Type 10 cement in a humid

environ ment. The silica fume must play a certain role in the mix

since it reduces the expansion compared to ordinary Type 10

Portland cement (at 200 C).

• The cements containing blastfurnaced slag (Spinor A 12 and

MC500) shrank more than ordinary Portland cements.

108

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0.12 -~ 0 0.09 -c:

0 cn 0.06 c cu a. 0.03 x ~ Q) 0 Cl cu ~ c -0.03 'C .c (J) -0.06

0 5 10 15 20 25 30 Curing time (days)

' ..... Type 10 * Type 30 ~Type 10SF ... MC500+SP 1

0.06 -~ 0 -c 0.03 0 fn c cu C- O

~ Cl

-0.03 cu ~ c:

ï:::: .c (J) -0.06

0 5 10 15 20 25 30 Curing time (days)

I--Type 10*650SR -9-900 ... A12 ."!l-E12

Fig. 7-12 Shrinkage/expansion at a temperature of 20°C and relative humidity of 100%

109

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-'#. 0 -.§ -0.1 (/)

~ -0.2 t====::~;~~;;~:::::!~~~~~;~:l ~ -0.3 Ci> g> -0.4 +-------------~ ...... --___4 __ ..

~

.§ -0.5 +------------------~

.c CI) -0.6 +---+----1~_+__+-+___+_____4f__+__+-+__+___I

o 5 10 15 20 25 30 Curing time (days)

,-Type 10 "* Type 30 -9- Type 10SF ... MC500+SP 1

.-~ 0 .. ==========~----------------_1 -5 -0.1 "in

~ -0.21==:§;:::::~~==::~~;;~ ~ -0.3 Ci) ~ -0.4 t--------=~~~ ...... Ii:=::::~=-===~d

.::.t:.

.~ -0.5 -1-------------------:: .. ------4"

.r::. en -0.6 +---t--+---+-____4~_+__+-_+__+-+__-t--~_t

o 5 10 15 20 25 Curing time (days)

I_Type 10* 650SR -9-900 ... A12 ..... E12 1

Fig. 7-13 Shrinkage/expansion at a temperature of 200C and relative humidity less than 30%

110

30

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• Ultrasonic pulse velocity

The u/trasonic pulse ve/ocities (Figs. 7-14 and 7-15) and the dynamic constant values (Ed in Figure 7-16) are also presented in Tables H-1 to H-4 (Appendix H). They are given as a function of effective W/C ratios.

A number of trends can be observed:

• Of ail the cements tested in this study, Type 10 grout specimens genera"y have the lowest pulse velocities, using the effective W/C ratio for comparison purposes.

• On average, Type 30 cement grouts have higher pu/se veloeities than the reference Type 10 r,ement grout.

• The dynamic modulus of elasticity values obtained with this test are, on average, 15 to 25% higher than the ones obtained with the destructive test. But the same tendeneies were noticeab/e; the irtermediate and microfine cement grouts give higher values for the dynamic modulus of elasticity than for the reference Type 10 grouts.

III

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• 4000 • lit -.!!! 3000 E -'0 cD

{~:r tljfSR

cD ~ II)

2000 cD >

Il L.nko 731

; "-cu cD .r:. 1000 en -'

o • 1 •

1 1 1

0.40 0.50 0.60 0.70 0.80 0.90 Effective W/C ratio

• 4000 • tif -II) 3000 -E -'0 cD cD ~ II)

2000 cD >

DA16

§+SP _AI2

SptnOf E12

cu ~ -.. cu cD .r:. 1000 Cf)

a • • • 1 1 1 1

0.40 0.50 0.60 0.70 0.80 0.90 Effective W/C ratio

• Fig. '-14 Shear (transversal) wave speeds at 20°C

112

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4000 -r---------=--------.==:;,

~ --g 3000 CD a. C/)

CD > ~ c: o 'in CI)

~

2000

~ 1000 o ()

-CI) --E -"C CD CD Q. CI)

CI) > cu ~ c: 0 'in CI)

! Q. E 0 ()

4000

3000

2000

1000

0

0.40

1

:>.40

0.50 0.60 0.70 0.80 0.90 Effective W/C ratio

• fit OA16 _.SP IIA12

1- SptnorE12

.-

. 1. 1 . • • . 0.50 0.60 0.70 0.80 0,90

Effective W/C ratio

L--______________________________________________ _

Fig. 7-15 Compression (longitudinal) wave speeds at 20°C

113

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25

Cà 20 a.. (!) -Z;> ë3 15 :.;l CIl l'ti Q; .... o 10 CIl ::J "3 ~

~ 5

o

25

Cà 20 a.. (!) ->. 13 15 :.;l CIl l'ti Q; .... 0 10 CIl ::::J :; "0 0

5 ~

o

I 1 . . . 0.40 0.50 0.60 0.70

Effective W/C ratio

L 1 ~ 1

0.40 0.50 0.60 0.70 Effective W/C ratio

Fig. 7-16 Dynamic modulus of elasticity at 20°C

114

• If [~r frffSR -- -

~ lanko 737

r- f-- r-

0.80 0.90

• 1)'° 0: E:j'A16

E:f+SP 1- lirA12

Sptnor E12

0.80 0.90

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• Permeability

The permeability index gives interesting informations on the hardened grout durability (23].

Analysis of the permeability test data can be summarized as follow:

• Ali of the cements tested in this study were found ta be almost perfectly impermeable since the permeability index was less than lx10-11 cm/s for a maximum pressure differential of 13 MPa (no water went through the hardened grout specimens, even after being subjected to this pressure for many days).

• Ali cement-based grouts (ordinary Portland cements and Mes) must then be homogeneous, dense and contain very few microscopie pores. The values given by Mehta [23J in Table 6-10 at ultimate hydration is 6x 10-11 cm/s.

Therefore, the permeability of ail cements is not affected by the variation of the initial W/C ratio in the range studied (W/C ratio between 0.4 and 2.0) .

• Microstructural characteristics

Following this analysis, Phatographs 7-1 through 7-4 were taken which show that the specimens are very dense and homogeneous and contain almast no pores. These observations were predictable in reality, because the permeability test had shown that ail specimens without exception were impermeable, thus containing very few pores.

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Photo 7-1 Type 10 cement with an initial W/C ratio of 0.8 (3500 X)

Photo 7-2 Type 30 cement with an initial W/C ratio of 0.8 (3500 X)

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Photo 7-3 Microcem 650SR cement with an initial W/C ratio of 0.8 (1100 X)

Photo 7-4 MC500+SP cement with an initial W/C ratio of 0.8 (2200 X)

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7.3 Effect of temperature

One of the main objectives in this study was to determine the effect

of tempe rature on the behavior of both fresh and hardened MC grouts used

for injection.

7.3.1 Fresh grout characteristics

• Viscosity

Viscosity results (Tables 8-1 and B-2, Appendix B) obtained at

different temperatures (40C, 100 C et 200C) are similar when the readings

are taken just after mixing.

However, for most liquids, the viscosity values increase when the

surrounding temperature is lowered (see Table 7-2) [28]. The results

obtained on the grouts may be explained as follows: the water used for ail

the grouts has a temperature around 150 C and the cement bags are stored

in the laboratory at approximately 200C (not in the climatic chamber

temperature) to effectively simulate the site conditions. The grout internai

temperature takes a while before stabilizing to a certain value that depends

on the surrounding tempe rature (climatic chamber's).

Table 7-2 Absolute viscosity of different liquids

Absolute viscosity (cps)

Temperature Water Mercury Ethylene-

glycol (oC)

4 1.57 1.60

10 1.31 > 30.0

20 1.00 1.55 19.90

The relative viscosity values (Figs. 1-1 to 1-18, Appendix 1) of cement­

based grouts change slightly with variation in temperature if they are taken

60 minutes after mixing. Two reasons explain this change: the heat transfer

between the climatic chamber and the specimens stabilizes after a period of

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60 minutes and the cement grains are hydrating and induces the grout to

set, thereby increasing its viscosity.

Table 7-3 (below) shows that even after one hour in the climatic

chamber, the internai temperature of the grout does not stabilize at the

surrounding temperature. The reason is that the hydration process induces

heat and the equi/ibrium temperature is a runction of time. The chemical

reaction between water and cement is exothermic, since heat is generated

which can last several hours, even days depending on the cement type and

the humidity level of the environment.

The grout temperature increases to 22°C when the ambient

temperature is set at 200C. However, it decreases to 70C and 11 0 C when

the tests are performed in a chamber where the ambient temperature is set

to 40C or 100e respective/y.

Table 7-3 Grout internai temperature variation vs. surrounding tempe rature

Grout average Grout average Climatic chamber ternperature just temperature temperature

after mixing 60 min after (OC) (OC) mixing (OC)

15 7 4

15 11 10

15 22 20

Thus, variations in the ambient temperatures will greatly influence the

hydration reaction between the cement grains and water: a lower

temperature slows down any exothermic reaction such as that between

cement and water [23].

The main observations concerning the effects of temperature

variations on the relative viscosity values of cement-based grouts are

summarized as follows:

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• Just after mixing, the different grouts have almost identical

relative viscosity values regardless of the ambient tempe rature

of the climatic chamber (40C, 100 C or 200C).

• The heat transfer process continues with time and affects the

grout viscosity because the hydration phenomenoo is

accentuated. Since the setting times of any grouts are shorter

when the ambient temperature is high, the viscosity values will

also rise over time.

• The viscosities of the coarse (Type 10 and 30), the intermediate

(Microcem 650SR and 900) and Lanko 737 cements change

only by variation of tempe rature one hour after mixing.

• The viscosities of the MCs (Spinors and MC500) are usually

higher after one hour with an increase of temperature at ;ow

W/C ratios. It should be noted that these cements set very

rapidly and this influences the viscosity quite rapldly with low

W/C ratios .

• Bleeding (stability)

Grout stability is verified after letting the grout rest for 120 minutes. If

less than 5% of bleed water has appeared on the surface, the grout is

defined as "stable". Figures J-1 to J-18 in Appendix J contain bar charts

showing the variation in the suspension volumes of ail cement grouts after

120 minutes and also in their final state for different ambient temperatures

(40C, 100C and 200 C).

To verify accurately the effect of a tempe rature variation on the grout

bleeding rate, the final state of bleeding reached by each MCs shows better

results than the ones take at 120 minutes because, as seen earlier, the

effect of the ambient temperature on the grout internai temperature takes

some time to stabilize. Depending on the cement type and the initial W/C

ratio used, the sedimentation process may take up to 600 min.

It may be seen in Table C-1 (Appendix C) and in Figures J-l to J-18

that the influerce of temperature variations is not significant and does not

affect the bleeding of fresh grout.

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Thus, it can be concluded that the grout stability is not affected by

tempe ratures

• Setting time

The temperature variation affects significantly the graut setting times,

as seen in Figures K-1 to K-20 in Appendix K. The reason is that the ambient

temperature slows down or accelerates the hydration reaction process

(exothermic reaction) as the temperature is lowered or raised, respectively.

Mehta (23) explained the generation of hydration heat by studying the

cement grout with a calorimeter to measure the rate of heat liberated during

the first 24 hours of curing. Fig. 7-17 shows two peaks in the first 24

hours: the descending peak A represents the initial setting time (beginning of

solidification and stiffening), whereas ascending peak B represents the final

setting time (complete solidification and beginning of hardening) of the

graut .

. a 1 2 ... o

!! 1 a

a::

O~~~--~-L~L-~ o 4 8 12 16 20 24

Tlme • Hours

Fig. 7-17 Rate of heat liberation (23)

The principal conclusions regarding temperature effects on the grout

setting times may be summarized as follows:

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• An increase in temperature (Figures K- 1 to K-20) reduces the

setting times for ail cement and MC-based grouts tested. At low

W IC ratios, the difference (time) between the three curves is

not significant, however it increases significantly as more water

is added ta the mix.

• The initial setting times for Type 10 cement grout at 40 C vary

from 15.5 h ta 23.2 h for initial W/C ratios ranging from 0.4 to

0.8. The initial setting time decreases drastically (more than

50% in certain cases) when the temperature is raised to 200 C.

• The initial setting time of Type 30 cement graut is also much

shorter when the temperature is raised fram 40C to 200 C. Tests

at the intermediate temperature used in the study (100C)

showed that the initial setting times for Type 30 cement

decreases by almost 30% compared to the values at 40 C. As

stated earlier in Section 7.2.', the fineness and chemical

composition are the main causes for these shorter times.

• For ail MCs, an increase in the curing temperature fram 40 C to

200 C reduces the setting time to different degrees. MCs

(without SPI always have shorter setting times than those

obtained with Type , 0 cement, which confirms that fineness

plays an important raie in the setting-time of cement based

grout [19].

Thus, the main conclusion is that a decrease in temperature results in

longer setting times for ail types of cement grouts, and vice-versa. It is

suggested that, if reasonable setting times are desired, an injection should

be undertaken when the ambient temperature is at least l00 C.

7.3.2 Hardened graut characteristics

This section focuses on the effect of curing temperature (40 C, 'OoC

and 200 C) on the physical characteristics of MC-based grouts .

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• Modulus of elasticity

Figures L-1 to L-6, in ApJJendix L, show the influence of temperature

on the modulus of elasticity (E) as a function of the initial w/e ratio for each

cement.

It proved almost impossible to measure the values of the modulus of

elasticity, E, and the Poisson's ratio, u, when cured at 4°C and 10°C on the

three blended-Portland cements containing granulated blast-furnace slag

(MC500, Spinor A 12 and A 16) with and without superplasticizer. The

cylindrical specimens were very friable and crumbled after a short period of

time (Iess than one hourI when removed from a moist environment. It seems

that the exterior surface was drying-out (Ioosing its water content by

evaporation) whereas the interior core remained humid (and still solid). Thus,

tensile stresses are appearing on the surface and multiple microcracks make

the specimens impossible to test .

Since the phenomenon appeared regardless if SPs were used, the

effect of this type of admixture can not be pointed out specifically as being

a cause of the problem even if it is weil known that some SPs are not

efficient when the temperature is below 100 e [4, 5, 11, 25].

However, this phenomenon was almost not observed when these

specimens were cured at 20°C. Maybe the blended-Portland (with blast

furnace slag) are almost completely i1ydrated after 28 days at that

temperature and the need of water is minimal then. It is known that blended­

Portland cements with blast-furnace slag take more time to both hydrate and

gain strength than ordinary Portland cements [4, 22].

It can be seen that the temperature cannot be neglected as a

contributing factor ta the strong variations in the values of E and u of the

different hardened grout specimens. The general tendencies observed can be

summarized as follows:

• At 40 C, the values of E are always the lowest for ail grouts.

This confirms that at low temperature, the hydration reaction

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..-... cu a. C> ->. +oJ

'0 ~ fi) cu Ci) '-0 fi) ::::l ::::l '0 0 ::;

between cement and water is slowed down and, at the same

time reduces the strength of the hardened product.

• However, it was noted that 4 cements (Type 10, Type 30,

Microcem 650SR and 900) which were cured at the three

selected temperatures (40 C, 100 C and 200C) reached the

maximum compressive strength values when cured at 1 DoC,

and not as expected at 200C. Therefore, there exists an

optimum curing temperature at which different grouts develop

their physical properties to an optimum level (se.~ Fig. 7-18, for

example). This phenomenon was also noted by Mnif [381 during

his studies at the Sherbrooke University.

• In general, the Poisson's ratio (v) follows the same trend

(maximum values at the same optimum temperature) as the

modulus of elasticity; these values vary between 0.10 and 0.17

for the different MC grouts.

20 Initial W/C = 0.6

15

10 ..

5 0 5 10 15 20 25

-&900

Fig. 7-18 Modulus of elasticity vs. curing temperature

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• Compressive strength (fe')

The cu ring temperature has the same effects on the compressive

strength of the hardened grout specimens as on the modulus of elastieity.

No values could be determined at 4°C and 10°C for the three cements

containing granulated blast-furnace slag (MC500, Spinor A 12 and A 16). The

friability (crumbly) problem experienced with these cements prevented us

from studying the effect of the temperature on fc' as for E. The moisture

level, the curing temperature, curing period and SPs used are probably the

factors which greatly influence this type of cement.

Since no problem was encountered when testing Lanko 737 at 4°C,

this blended-Portland cement probably does not contain as much slag .as the

other similar cements (MC500, Spinor A 12 and A 16) or it does not contain

slao at ail.

Close examination of the Figs. M-1 to M-6 (Appendix M) reveals the

following effects of tempe rature variation on the compressive strength of

hardened grouts:

• The compressive strength, fc', values at 40 C are always the

lowest obtained for ail grouts tested (the same conclusion as for

the modulus of elasticity).

• The same four cements used in the previous tests (i.e. Type 10,

Type 30, Microcem 650SR and 900) are more resistant in

compression when they were cured at 100 C (not as expected at

200 C). Therefore, there is an optimum curing temperature for

each cement (see Fig. 7-19).

• It is important to use the lowest initial VV IC ratio (for ail types of

cements) possible because grout strength (compressive) in the

hardened state is greatly affected by the W/C ratio used.

Therefore, the same conclusion apply for both the rnodulus of

elasticity and the compressive strength characteristics: cements have an

125

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optimum curing temperature. For coarse and intermediate Portland cements,

it appears that this optimum temperature is near 1 Qoe.

Initial W/C = 1.0 20~-----------------------------------

~ 10+-------~~--------------~----~

o 5 10 15 20 25

-&900

Fig. 7-19 Compressive strength vs. curing tef"lperature

• Shrinkage/expansion

The linear shrinkage/expansion test was performed during the first

month of curing of the hardened grout specimens. The influence of

temperature on the shrinkage characteristic was studied using two

temperatures (40 e and 200 e) and the results are presented in Figs. N-1 to

N-B (in Appendix N). It should be noted that the expansion process has

positive values whereas the shrinkage process is represented by negatlve

values.

ln many cases (except MC500 + SPI when the specimens are in a

humid environment it can be seen that a low temperature increases the

expansion process.

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On the other hand, when the environment is not humid, the

temperature variation affects the grouts in different ways, depending on the

graut type. Type 10 and Type 30 cements, for instance, shrink more when

the temperature is low, whereas the others (Type 10SF and Spinor A 12)

shrink more at higher temperature.

Thus, the effect of temperature variation is dependent on the cement

composition and type (Portland, blended-Portland slag, admixture added,

etc.) since their coefficient of thermal expansion is different .

• Permeability

The permeability of the grout specimens is not affected by

temperature changes: ail specimens are still almost perfectly impermeable

(as mentioned in Section 7.2.2), regardless of the cu ring temperature .

• Ultrasonic pulse veJoeities

The pulse veloeities (compressive type and shear type) are affected by

curing temperature variation. The data obtained trom this test is presented in

Figs. 0-1 to 0-12 (Appendix 0). It may be concluded that a low temperature

(40 C) affects most of the cement grout specimens negatively (velocities are

slower, indicating it is less dense and more porous). It is, therefore,

preferable to use these products when the temperature is at least 100C ta

obtain acceptable physica! characteristics.

It should be noted that sorne of the values obtained and shown in the

Figures are sometimes too high or to low because on sorne occasions the

wave signal was difficult to perceive when it went through the hardened

specimens.

As for the other tests for the mechanical properties, the fastest

speeds were generally obtained for the specimens which were cured at a

temperature of 10°C .

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7.4 Effect of chemical ad mixtures

The two chemical admixtures tested in this program are the

superplasticizers (SP) and the anti-washout agents (AWA). Superplasticizers

(SP) are products designed ta Improve both the viscosity and the bleeding

(stability) of a graut, although they have the disadvantage of increasing the

setting time. Anti-washout agents (AWA) are designed to mainly reduce the

washout rate of fresh graut in a crack by water (pressure and velocity) and

decreases the graut bleeding rate (increasing its stab,lity).

The sections that follow describe only the effects of SP and AWA on

the rheological characteristics of grouts.

7.4. 1 Superplasticizers

The three rheological characteristics of the grout (viscosity, bleeding,

setting time) were examined for each graut mix at a temperature of 20°C.

Type 10 cement was used as the reference and tested with a naphthalene­

based SP (Eucon from Euclid Inc.) and a melamine-based SP (Melment also

from Euclid Inc.). The three Spinor MCs were also mixed with the Melment.

The SP proportions used (dry weightl are always expressed in terms

of the weight of the cement used for the initial W IC ratio. The MC500

cement is mixed with its own SP (NS200) in a proportion of 1 % with

respect to the weight of the cement. Lastly, the SP proportion in the Lanko

737 was unknown because it was already added in powder form in the

cement by the manufacturer .

• Viscosity

The addition of SP in any quantity to the grout mix is aimed mainly at

reducing its viscosity (or increasing its fluidity). Figures 7-20 to 7-24 present

viscosity data for different MC grouts relative to a reference Portland cement

Type 10 .

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500 Naphthalene-based SP ...

Type 10 - 400 -V-tn Type 10+SPIO.2%1 a. 0 * - Type 10+SPIO,4%) ~ 300 .... 'in Type 10+SPI1.2%1

8 ... tn Type 10+SPI2.0%1 '> 200 Q)

> .. al "i 100 Q:

o 0.5 1 1.5 Initial W/C ratio

Fig. 7-20 Relative viscosity of Type 10 cement with a naphthalene­based SP at 20°C

500 Melamine-based SP ...

Type 10 - 400 -V-tn a. Type 10+SPIO.3%1 0 * -~ Type 10+SP(O.6%1

'0 300 ... 8 II

Type 10+SPC1.0%1 ... U) , Type 10+SP(1.5%1 'S \ Q) 200

\\ > .. al "i 100 Q:

~~ • 0 0 0.5 1 1.5

Initial W/C ratio

Fig. 7-21 Relative viscosity of Type 10 cement with a melamine­based SP at 20 ° C

129

2

2

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500 -Type 10 - 400 ...... tn Q. A12 0 "* -~

A12 + SPI1.2%)

en 300 ... 8

A12 + SP(4.0%1

tn '> 200 Q)

> ~ lU 1) 100 IX:

0 0 0.5 1 1.5

Initial W/C ratio

Fig. 7-22 Relative viscosity of Spinor A 12 MC with a melamine­based SP at 20 0 e

500 .. Type 10

- 400 ......

tn A16 Q. 0M-O

2

- A16 + SP(1.2%1

~ 300 ...

'in E12

8 .. fi) E12 +SP/l.2%)

'> 200 Q) > ~ lU Qi 100 0:::

0 0 0.5 1 1.5 2

Initial W/C ratio

Fig. 7-23 Relative viscosity of Spinor A 16 & E 12 Mes with a melamine­based SP at 200 e

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500 ... Type 10 - 400 09-", MC 500 +SP C.

0 -M-- lanko 737 ~ "in 300 8 ", 'S;

200 CD > :.e::; as ëD 100 ~

o 0.5 1 1.5 2 Initial W/C ratio

Fig. 7-24 Relative viscosity of MC500+SP and Lanko 737 MCs at 20°C

The previous graphs show that SPs reduce the v.scosity of cement­

based grouts:

• Naphthalene-based SP, with a proportion of 1.2°A, (dry weight)

per cement by weight, considerably reduces the grout viscosity

when the initial W/C ratios are small. However, a proportion of

2.0% of SP does not make any significant difference compared

with a proportion of 1.2% of SP which appears to be the

optimum quantity.

• Melamine-based SP is used optimally when its proportion, per

cement by weight, is near 1.0%. It was noted that a croportion

of 1.5% of this SP did not significantly change the viscosity

readings .

• SP substantially lowers the relative viscosity values of MC

grouts. With 1.2% of melamine-based SP used with Spinor A 12

and A 16, th'=! relative viscosity is nearly 50 times lower than the

value for an initial W/C ratio of 0.8. In the case of Spinor E12

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with SP, the relative viscosity values also decrease for ail W/C

ratios.

• MC grouts used without any SP do :",ot have good fluidity until

very high W/C ratios. Therefore, SP must be used if high fluidity

is required (thus low viscosity), it also has a favorable effect on

the mechanical properties of the grout since less water is

needed for a specific viscosity.

• The naphthalene-based SP produces a lot of air bubbles in the

grout mix .

• Bleeding (stability)

The addition of SPs (Figs. 7-25 to 7-28) is also intended to improve

the stability of the grout, since these products deflocculate the cement

grains in suspension in the water.

However, if too much SP is used in the mix, the grout may becorne

over-saturated, which would increase the segregation of grains and cause

more bleeding compared with the condition when no SP is used. It is,

therefore, essential to determine the optimum quantity (which is a function

of cement weight) of SP for each initial W/C ratio to be used during the

injection.

It can be concluded that:

• The addition of a SP (melamine- and naphthalene-based) does

not influence the bleeding rate of Type 10 cement with an initial

W/C ratio of 0.4. However, a small proportion of SP (0.2%

Eucon or 0.3% Melment) slightly improves the stability (reduces

the bleeding rate) of Type 10 cement grout when the initial W/C

ratio is high.

• In fact, the stability of a grout would be increased in the sense

that, for a given fluidity, less water is required with the addition

of SPs, thereby reducing the W/C ratio .

• When the Type 10 cement grout has medium or high initial W/C

ratio (1.0 and 2.0), a proportion of SP exceeding 0.2% (Eucan)

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-~ ° -Q)

E ::l '0 > c 0 fn c Q) Co U) ::l

C/)

or 0.3% (Melment) over saturates the grout and causes

considerable bleeding of water on the surface .

• A SP added to a MC (Spinor A 12, A 16 and E12) does not

change their stability results for any initial W/C ratios. It should

be noted that these MC grouts are stable even without SP

agents at high W/C ratios. New tests performed at very high

W/C ratios (3.0, 4.0, 5.0, etc.) should be performed to verify if

SPs have an effect on their bleeding rate.

Type 10 + SP(naphthalene) 100

80

60

40

20

0 0.4 1.0 2.0

Initial W/C ratio

1_(O.OO/OSP) ~(O.2% SP)D(O.4% SP)fB(1.2% SP)~(2.00/0 SP)1

Fig. 7-25 Suspension volume of Type 10 cement with a naphthalene­based SP at 20°C

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-'#. -Q)

E :l (5 > c o "ii) c Q)

100

80

60

40

~ 20 :l en

o

Type 10 + SP(mellmine)

0.4 1.0 2.0 Initial W/C ratio

1_(0.0% SP) ~(O.3% SP) 0(0.6% SP) .(1.0% SP) ~(1 5% SP) 1

Fig. 7-26 Suspension volume of Type 10 cement with a melamine­based SP at 20°C

100 -cf!. 80 -Q)

E :l 60 (5 > c

40 0 .;;; c Q)

20 c... t/) ::::J en

0 0.4 0.5

_Type 10 F1JA16

0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

~E12 DE12+SP(1,2%) ~A16+SP(1,2%)

Fig 7-27 Suspension volume of Spinor A 16 and E12 MCs with melamine­based SP at 20°C

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-~ o -Q)

E :::s a > c: a U) c: Q) c­U) :::s en

100

80

60 -+-==1--

40

20

o 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

.Type 10 ~A12

DA12 + SP(1,2%) ~A12 + SP(4,O%)

Fig. 7-28 Suspension volume of Spinor A 12 MC with a melamine­based SP at 20°C

• Setting time

The superplasticizers are known to increase the setting times of

cement-based graut [11]. Figures 7-29 to 7-36 show the initial and final

setting times for different grouts to which SPs were added in different

proportions. The following observations were made after completion of this

test:

• Both types of SP (melamine and naphthalene) strangly affect

the initial and final setting times of Type 10 cement grout by

increasing significantly the time for hardening. Therefore, a

melamine-based SP should not be used with a proportion

greater than 0.6% whereas a naphthalene-based should be set

ta 0.4% for the range of initial W IC ratios used.

• SP also increases the setting times of Spinor A 12, Spinor A 16

and Spinor E12 .

135

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30

25

- 20 en ~

::J 0

oC 15 -Q)

E .- 10 t-

5

0

Type 10 + SP(naphthalene)

-+-_______________ ~ (0 C'/eSP)

-9-(02% SP)

+-------------~------~~ (04% SP) ...

+-------~.",c...~~~""""------~ (1 2% SP) -& (20% SP)

0 0.5 1 1.5 Initial W/C ratio

Fig. 7-29 Initial setting time of Type 10 cement with naphthalene­based SP at 20°C

2

Type 10 + SP(naphthalene) 30 T-------------------~~---------------------------~ -25 +-______ ~~-------~(OO%SP)

.sr (02% SP)

- 20 +--------------~~------.......... -----~"* I!! ~ (04% SP) o é15 ... d) (12% SP) E & j:: 10 (20% SP)

5 +----------------------------------------------------------------------~

o +-+-~~-+-+--+-~+-~~~-+--+-~~~+-~-+-+~ o 0.5 1 1.5

Initial W/C ratio

Fig. 7-30 Final setting time of Type 10 cement with a naphthalene­based SP at 20°C

136

2

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..

Type 10 + SP(melamine) 30r---------------------~~==~ -25 +------------------------f (00% SP)

-9-(03% SP)

W20 +---------------.--.--------t* :::J (06% SP)

o * é 15 (1.0% SP) ~ ~

.5 1 0 (1.5% SP)

.....

5+-------------------------------------~

o~~~+-~~+-~~+-~~~~-+~~~~

o 0.5 1 1.5 Initial W/C ratio

Fig. 7-31 Initial setting time of Type 10 cement with a me/amine­based SP at 20°C

30

25

- 20 ~ :::J 0 .c 15 -~ E .- 10 .....

5

0

Type 10 + SP(melamine)

-+----------J'---J;""....-----------f (00% SP) .. (0.3% SP)

+----------+~----~----------f* (06% SP) ....

+------+-+-~~~---------f (1 0% SP)

0 0.5 1 Initial W/C ratio

1.5

-& (15% SP)

Fig. 7-32 Final setting time I)f Type 10 cement with a me/amine­based SP at 20°C

137

2

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30 .. 25

Type 10

• MC500+SP

"* - 20 Llnko 737 [!? .. ::l 0 E 12

.s=. 15 .. --CD E12+SP(1.2'11t)

E 10 i-

5

o L-+-__ ~==~ __ +-__ ~ __ +-__ +-__ ~ 0.4 0.5 0.6 0.8 1 1.2 1.5 2

Initial W/C ratio

Fig. 7-33 Initial setting time of MC500+SP(NS200), Lanko 737 and Spinor E12 + SP(melamine) at 20°C

30 ... 25

Type 10 ..... MC500+SP -Mo - 20 Lanko 737 [!? ...

::l E 12 0

.&:: 15 .... -CI) E 12+SP(1.2'11t)

E 10 i=

5

0

0 0.5 1 1.5 2 Initial W/C ratio

Fig. 7-34 Final setting time of MC500+SP(NS200t, Lanko 737 and Spinor E12 + SP(melamine) at 20°C

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30 ... 25

Type 10 09-A 12

"* - 20 A12+SP(1,2'11o) ~ ..-::J

A16 0 .c 15 .. - A16 +SP(1,2'11o) Q)

E 10 t=

5

0 0 0.5 1 1.5 2

Initial W/C ratio

Fig. 7-35 Initial setting time of Spinor A 12 and A 16 with a melamine­based SP at 20°C

30 ... 25

Type 10 09-A 12

"* - 20 A12tSP(1.2'11o) ~ .... ::J

A 16 0 .c 15 .. "-" Q)

A16 +SP(1.2'11o)

E 10 ;::

5

0 0 0.5 1 1.5 2

Initial W/C ratio

Fig. 7-36 Final setting time of Spinor A 12 and A 16 with a melamine­based SP at 20°C at 20°C

139

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7.4.2 Anti-washout agents

Two anti-washout agents (AWA) were tested: Sikament 100SC (liquid

form) produced by Sika and Walan Gum (powder form) distributed by

Ciment St-Laurent .

• Viscosity

Figure 7-37 contains the relative viscosity curves of Type 10 cement

grouts with AWA as a function of the initial W/C ratio.

500 -Type 10 - 400 .sr ri) Tl0+Slka 100SC a. 0 "* - Tl0+Welan Gum ~ .- 300 ri) 0 0 ri)

'> 200 ~

+=i CU

Q) 100 0::

0 0 0.5 1 1.5

Initial W/C ratio

Fig. 7-37 Relative viscosity of Type 10 cement grouts with AWAs at 20°C

2

The analysis of the previous Figure (7-37) show that the AWAs

significantly increase the relative viscosity of the Type 10 cement graut,

especially at low W/C ratio. It would be preferable if a compatible SP is also

used to obtain acceptable viscosity values for a given fluidity (viscos:ty).

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• Bleeding (stability)

The bar chart in Figure 7-38 presents the suspension volume of Type

10 cement grouts with AWAs. The values were taken 120 minutes after the

grouts were mixed.

100

-~ 80 (l)

E :J 60 ~ c:

.Q 40 fi)

c: (l)

0. 20 fi)

:J CI)

o 0.4 1.0

Initial W/C ratio

~T10+Sika 100SC(]T10+Welan GU3

Fig. 7-38 Suspension volume of Type 10 cement grout with AWAs at 20°C

As specified in the manufacturer's technical data sheets, the AWAs

reduce the bleeding of water on the top surface of the grout.

The use of Sikament 100SC and Welan Gum AWA made the Type 10

cement grout stable with an initial W/C ratio of 1.0. The Welan Gum AWA

also made the grolJt stable at an initial W le ratio of 2.0. Therefore, the use

of AWAs is clearly a good way of improving the grout stability (reduces

bleeding).

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• Setting time

According ta the AWA manufacturers, the grout setting time is the

rheolagical property which is most affected by the addition of the AWA

(Figs. 7-39 and 7-40).

These manufacturers (and distributors) also specify that these

products (AWAs) shauld be used when the ambient tempe rature is higher

than Boe, otherwise the setting time is very long.

It can be concluded that the setting times of Type 10 cement grout

increases when the Welan Gum AWA is added and does not change with

the Sika product.

30

25

- 20 ~ ::J 0

15 oC -Q)

E ~ 10

5

0

... Type 10

+-------------------------~~ T10+Slka 100SC

~----------------~------~~ T10+Welan Gum

0 0.5 1 1.5 Initial W/C ratio

2

Fig. 7-39 Initial setting time of Type 10 cement grout with AWAs at 20°C

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30 -25 Type 10 ...... n O+Slka 100Se - 20 *" ~ nO+Welan Gum

:::::J 0

15 .c ........ Q)

E 10 i=

5

0

0 0.5 1 1.5 Initial W/C ratio

Fig. 7-40 Final setting time of Type 10 cement grout with AWAs

at 20°C

• General conclusions

2

ln conclusion, the effects of AWAs on the rheological properties of

cement grouts may be summarized as follows:

• The A WAs significantly increase the viscosity of Type 10

cement grout, and the use of SPs is recommended to lower

such high viscosities.

• The bleeding rate is lower when an AWA is used.

• Certain AWA increases the setting times of Type 10 cement

grout .

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7.5 Effect of mixing

The main parameters to be checked are the mixing speed and time

used for preparing a cement grout with the mixer. It has becn observed that

the speed variation affects certain MC grout properties [16].

To verify the effect of the mixing time, several grouts were prepared

with Type 10, Type 30 and Type 10SF (8% silica fume by weight) cements

at a temperature of 200C.

7.5.1 Mixing time

The mixing procedure was the same for each grout: three initial W/C

ratios were selected (0.4, 1.0 and 2.0) and the grouts were mixed at a

speed of 2300 revolution per minute (RPM). On the other hand, the time

d uration varied between 1, 4, 10 and 15 minutes. The three rheological

properties (viscosity, bleeding (stability) and setting time) were tested using

the standard procedures.

• Viscosity

The data obtained is shown in Tables 7-4 and 7-5 and in Figs. P-l to

P-6 (Appendix Pl. The relative viscosity values presented here were recorded

just after and 60 minutes after mixing.

Table 7-4 Relative viscosity for different mixing times taken just after mixing

Relative viscosity (cps)

Cement Type 10 Type 30 l"~e 10SF

Mixino

time 1 4 10 15 1 4 10 15 1 4 10 15

(minI

0.4 271 274 283 299 408 399 448 537 330 254 344 371

W/C 1.0 21 20 21 22 36 33 37 38 39 41 40 37

2.0 3.2 3.1 3.1 4.0 5.0 5.4 5.5 5.7 7.3 6.1 5.8 6.3

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Table 7-5 Relative viscosity for different mixing times 60 min after mixing

Relative VISCOSlty (cps)

Cement Type 10 Type 30 T~e 10SF

Mixing

time 1 4 10 15 1 4 10 15 1 4 10 15

(min)

').4 ---. 286 351 346 375 532 482 485 638 409 263 453 397

W/C 1.0 35 34 34 26 65 61 50 50 49 50 46 45

2.0 4.8 4.5 4.5 6.1 7.8 7.4 6.8 8.7 6.5 6.3 5.9 6.1

It can be seen that the influence of different mixing durations (from 1

to 15 minutes) does not significantly change the relative viscosity values of

the Portland cement based-grouts (especially and low W/C ratios). It should

be noted here that a high shear speed of 2300 RPM was used; different

results may be obtained if a slower speed is used .

• Bleeding (stability)

Table 7-6 and Figures P-7 to P-9 (Appendix P) present bar charts in

which the suspension volumes of the cement grouts are functions the initial

W/C ratios selected for the different mixing durations (120 minutes after

mixing).

Table 7-6 Volume in suspension for different mixing times 120 min after mixing

Suspension volumes (% 1

Cement Type 10 Type 30 Type 10SF

Mixing 1 4 10 15 1 4 10 15 1 4 10 time

(minI

15

0.4 100 100 100 100 100 100 100 100 100 100 100 100

W/C 1.0 73 81 80 78 83 82 81 82 94 95 83 88

2.0 51 50 47 48 64 67 70 73 55 62 63 64

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It can be concluded that the effect of mixing time, with a rotational

mixing speed of 2300 RPM, does not affect significantly the stability of any

grouts.

• Setting time

The data for the setting times of the cement-based grouts is presented

in Tables 7-7 and 7-8 and in Figs. P-10 to P-15 (Appendix P).

Table 7-7 Initial setting time for different mixing times

Setting time (hours)

Cement Type 10 Type 30 Type 10SF

Mixing 1 4 10 15 1 4 10 15 1 4 10 15

time

(min)

0.4 6.3 5.3 5.2 5.0 3.8 3.8 3.6 35 57 6.0 53 50

W/C 1.0 9.2 83 7.8 7.4 7.7 7.2 6.5 6.4 11 6 103 98 925

2.0 > 24 > 24 > 24 > 24 > 24 > 24 > 24 > 24 > 24 > 24 > 24 > 24

Table 7-8 Final setting time for different mixing times

Setting time (hours)

Cement Type 10 Type 30 Type 10Sf-

Mixing 1 4 10 15 1 4 10 15 1 4 10 15

time

(min)

0.4 7.3 6.7 6.7 6.0 48 4.6 46 4.4 68 7.6 6.4 6.0

W/C 1.0 16.8 15.2 15.0 12.0 12.7 13.7 113 11.0 160 17.3 13.7 13 1

2.0 > 24 > 24 > 24 > 24 > 24 > 24 > 24 > 24 > 24 > 24 > 24 > 24

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The important points to be noted are:

• The initial setting times for Type 10 (initial W/C = 0.4) cement

vary slightly from 6.3 hours to 5.0 hours when the mixing time

increases from 1 to 15 minutes. This is because when the grout

is mixed for a longer period of time, its cement grains have a

better chance to hydrate, thus produce more heat and reduce the setting time.

• However, the effect of mixing time for Type 10 cement is less

significant when comparing mixing durations such as 4 and 10

minutes.

• The same behavior was noted for the other cements (Type 30 and Type 10SF).

• General conclusions

The general conclusion to be drawn regarding the mixing time effects

on the rheological properties of cement grouts is that only the setting time is

slightly affected. Considering the sma" variation in setting times when the

mixing time is set to 4 minutes or 10 minutes, this range should be used

when the rotation al speed is equal to 2300 RPM.

7.5.2 Mixing speed

ln this section, the mixing time is kept constant (4 minutes) whereas

the rotational speed varies between 750 and 6000 RPM. The same

rheological properties as tested in 7.5.1 were verified (viscosity, bleeding (stability) and setting time).

• Viscosity

Some investigators, such as Schwartz and Krizek [16J, have

discovered that the rotational speed can influence certain rheological properties of MC-based grouts.

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The tests performed in the present study verify the effects of speeds

mixing on ordinary Portland cements. Tables 7-9 and 7-10 and Figs. Q-1 to

Q-6 (Appendix Q) contain the data obtained using the Brookfield apparatus.

Table 7-9 Relative viscosity for different mixing speeds taken just after mixing

Relative viscosity (cps)

Cement Tvpe 10 Type 30 Ty[>e 10SF

Mixing

speed

(RPM) 760 1600 2300 3000 6000 760 1600 2300 3000 6000 760 1600 2300 3000

0.4 . 298 274 292 343 • 383 399 459 416 . 297 322 358

W/C 1 0 20 24 20 21 21 32 35 37 36 37 33 41 41 39

20 3.4 3.4 3.1 3.7 3.7 4.3 4.8 5.0 48 48 54 5.9 6 1 6.2

*: could not be mixed (speed too low)

6000

360

37

7 6

Table 7-10 Relative viscosity for different mixing speeds 60 min after mixing

Relative viscoslty (cps)

Cement Type 10 Type 30 Type 10SF

Mixing

speed

(RPM) 760 1600 2300 3000 6000 760 1600 2300 3000 6000 760 1600 2300 3000 6000

0.4 • 386 350 348 379 . 495 482 671 416 • 358 400 358 360

E/C 1.0 30 30 34 27 27 62 66 57 58 66 44 47 50 50 48

2.0 5.0 5 1 4.5 5.1 o 1 6.1 6.8 7.4 67 69 58 63 63 6 1 67

*: could not be mlxed (speed too low)

The relative viscosity has a tendency to increase slightly when the

rotational speed increases. This is because at higher speeds, the cement

grains are weil mixed and they hydrate better with water.

It is recommended that the mixing apparatus be powerful enough to

generate a rotation speed of over 750 RPM. Problems were experienced

when using a speed of 750 RPM to mix grouts with an initial W le ratio equal

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to 0.4: the graut was too thick and this decreased the mixer rotational

speed nearly to zero .

• Bleeding (stability)

The results obtained are shown in Table 7-11 and in Figs. 0-7 to 0-9

(Appendix a). The different ratational speeds used ranged from 750 to 6000 RPM.

Table 7-" Volume in suspension for different mixing speeds 120 min after mlxlng

Suspension volume (%)

Cement Type 10 Type 30 Type 10SF

Mixing 160 1600 2300 3000 6000 160 1600 2300 3000 8000 760 1600 2300 3000 8000

speed

(RPM) 0.4 • 99 100 100 99 • 100 100 100 100 • 100 100 100 100

1.0 77 E/C

17 81 83 80 83 81 82 81 80 87 89 95 95 96

2.0 47 50 50 49 48 64 64 67 71 72 58 68 62 66 65

*: could not be mixed (speed too low)

It can be concluded that the rotational-speed variation does not

significantly affect the bleeding rate of any grouts for the initial W/C ratios

tested .

• Setting time

This section describe~ the tests performed to verity the effect of

variations in the mixing speed on the cement graut setting times. The

following trends may be detected from Tables 7-12 and 7-13 and Figs. 0-10

to 0-15 (Appendix a) :

• The setting times of the three cement grouts (Type 10, Type 30

and Type 10SF) are usually shorter (for low initial W le ratios)

when the mixing speed is high and when the mixing time is set

to 4 minutes. The rotational speed influence how weil the grains

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are shear mixed with water and, in the case of high speeds,

helps the hydration process.

• However, when the initial W/C ratio is high (> 1.0), the setting

time variation is only slight for the different speeds.

Table 7-12 Initial setting time for different mixing speeds

Initial setting tlme (hours)

Cement Tvpe 10 Tvpe 30 TYlle 10SF

Mixlng

speed

(RPM) 760 1600 2300 3000 8000 760 1600 2300 3000 8000 160 1600 2300 3000 8000

0.4 . 57 53 55 55 . 38 38 38 37 . 60 60 60 68

W/C 1.0 9.0 83 83 85 83 70 70 72 68 68 106 100 103 100 98

2.0 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24

.: could not be mixed (speed too low)

Table 7-13 Final setting time for different mixing speeds

Final setting time (hours)

Cement Tvpe 10 T (pe 30 Ty 19 10SF

Mixing

speed

(RPM) 160 1600 2300 3000 8000 760 1600 2300 3000 8000 160 1600 2300 3000 8000

0.4 . 72 67 67 70 . 58 56 58 48 . 78 76 75 70

W/C 1.0 17 155 162 145 140 133 140 137 132 123 175 175 173 170 170

2.0 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24 >24

.: could be mixed (speed too low)

• General conclusions

It may, therefore, be concluded that the effect of the mixing speed is

minimal if the speed used is equal or greater than 1500 RPM, with a mixing

time of 4 minutes. A rotational speed of 750 RPM is not recommended if a

thick grout is desired (it will be impossic-Ie to mix). Again, this data may

change if the mixing time less than or exceeds 4 minutes.

ISO

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CHAPTER 8

SUMMARY AND CONCLUSIONS

8.1 Summary

The injection procedure used to strengthen or seal a hydraulic

structure such as a dam requires a thorough understanding of the design of

the structure, the types of loads to which it is exposed, and the ambient

environmental and climatic conditions. If the injection product used is

incompatible with the cracked material (concrete in the case studied here),

the injection will not be successful. It is, therefore, essential that utilities

know the characteristics of the selected repair products. Ordinary (coarse

Portland), intermediate and microfine (especially for microcracks sealing)

cement-based grouts must therefore be tested and analysed so that their

rheological and mechanical properties can be determin~d .

Portland cement-based grouts at ambient temperature have already

been studied but microfine cements are relatively new on the North

American market and very little data is available for any temperatures (even

20°C). When manufacturers do provide information, it is for an ambient

temperature of about 20°C, but most dams and other concrete structures in

Canada are exposed to a much harsher and colder climate.

The main reason for using microfine cements for injection in hydraulic

structures is revealed immediately in their name: the grain size of these

cements is infinitely finer than for ordinary Portland cements. In fact, grouts

made of the latter simply cannot be injected successfully into cracks with an

opening smaller than 0.5 mm without forming a bridge or clumps

prematurely. Microfine cements, on the other hand, can infiltrate much

more easily into microcracks « 0.5 mm) and are more effective in sealing

the structure .

They have the major disadvantage, however, of having a much higher

viscosity than ordinary Portland cements. To reduce their viscosity, chemical

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agents such as SPs have to be added to the water-cement mix in various

proportions.

The injection conditions influence the choice of admixtures that can

be incorporated into the grout. For example, if the water flow is quite

considerable, anti-washout agents may be added to minimise the removal of

grout by the action of water. Also, low temperatures have a deleterious

effect on the grout setting time and the addition of a SP may have to be

considered.

8.2 Conclusions

A probing analysis of the results obtained from the many tests

performed in the course of this study validated the following points:

• The temperature affects only one of the rheological properties of

the graut; setting time. Furthermore, the temperature has an effect

on the mechanical characteristics of hardened graut. The ideal

curing temperature for Type 10-, Type 30-, Microcem 650SA- and

900-cement grouts is around 10°C (in order to get maximum

strength).

• Variations in the W le ratio have a substantial effect on the

following rheological and mechanical properties: viscosity, bleedirg

(stability), setting time, compressive strength, modulus of elasticity

and ultrasonic pulse velocities.

• There are two ways of reducing the viscosity of a grout: by

increasing the initial W IC ratio or using a SP. However, both

methods have inherent drawbacks:

- If the W/C ratio is increased too much, the grout becomes

unstable (excessive bleeding), its strength is decreased and it

takes longer time to set.

- If SPs are added, the setting time increases and there is a risk of

the grout oversaturing if the proportion of SP is too high. When

the point of equilibrium between the amount of cement and the

amount of SP is exceeded, the grout returns to a state of

instability caused by intensive bleeding.

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• Some cements become unstable when the W/C ratio is too high .

The result is that the final W/C ratio (also called "effective" or W/C

of "settled grout") is not the same as the initial W le ratio (at the

mixing stage).

• SPs are essential when microfine cements are used because

otherwise the resulting viscosity is too high. The choice of SP is

important, however, because it must be compatible with the

cements. Also, th'~ proportions used must be optimal since they

have a negative effect on some of the grout characteristics when

too much SP is mixed with the water and cement.

• Anti-washout agents (AWA) improve the grout capacity to avoid

being washed out by a flow of water. It was noted that they

increase the stability of the grout. On the other hand, these

products also increase the grout viscosity and a SP should always

be used with them.

• The effects of the mixing time (beyond 4 minutes) and mixing rate

(beyond 1500 RPM) are minimal (with a paddle mixer) on the grout

rheological characteristics .

• Most hydraulic blended-Portland cements with granulated blast­

fumace slag (Spinor A 12, A 1 6 and MC500 + SP) need more water

that ordinary cements for the sa me fluidity.

8.3 Future work

The aspects that cali for further study on some of the important

properties of cement-based grouts are listed below:

• The optimum temperatures for grout performance need to be

specifically determined. Future work should focus on temperatures

around 10°C.

• Several microfine cement products exist on the market.

Manufacturers quote excellent results with respect to certain

characteristics but regularly fail to mention other properties such as

stability, shrinkage/expansion, etc. They also rarely specify the

type and proportion of SP to use. The compatibility of the SP with

the cement used must be verified first and foremost, and then

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---------------------------------~-- - ------------ ---

optimum amount of SP should be used for the different W/C ratios

used for the injection.

154

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REFERENCES

1- Mirza, J., "Cracking in Concrete Dams: Causes and Remedies", Hydro­Review, Vol. IX, No. 3, June 1990, pp. 52-62 ..

2- ACI Committee 224, "Causes, evaluation and repair of cracks in concrete structures", Committee report No. 2241.R-84, ACI Journal, 1984, pp. 211-230.

3- Mirza, J., Popiel, M., Lacasse, J.P., Pelletier, M., Ballivy, G., Saleh, K., "Injectable cementitious materials for cracks in hydraulics structures", Proceedings ACI International conference Hong-Kong, 1991, pp. 217-231.

4- Houlsby, A.C., "Construction and Design of Cement Grouting", Wiley Series, 1990, 442 pp.

5- Saleh, K., "Rapport de synthèse et de re.;ommandation sur les méthodes, produits et équipement d'injection", IREQ-93-211, August 1993, 45 pp .

6- Karol, R.H., "Chemical grouting", Marcel dekker inc., Second edition, 1990, 465 pp.

7- Bruce, D.A., "Progress and Developments in Dam Rehabilitation by Grouting", Proceedings Conference on Grouting, Soil Improvement and Geotech., ASCE, New Orleans, La., 1992, pp. 601-613.

8- Clarke, W.J., "Performance Characteristics ol Microfine Cement", ASCE, Atlanta, Georgia, May 14-18, 1984.

9- Bruce, D.A., "The Practice and Potential of Grouting in Major Dam Rehabilitation", ASCE Annual Civil Engineering Convention, San Fransico, CA, November 5-8, 1990, 41 pp.

10- Hakansson, U., Hassler, l., Stille, H., "Rheological Properties of Microfine Cement Grouts With Additives", Proceedings Conference on Grouting, Soil Improvement and Geotech., ASCE, New Orleans, La., 1992, pp. 551-563,.

11- Ramachandran. V.S., "Concrete Admixtures Handbook: Properties, Science and Technology", Noyes Publications, 1984, 626 pp.

155

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12- Caron, C., "The state of grouting in the 1980's", Proceeding Conference on Grouting in Geotech. , ASCE, New Orleans, La., 1982, pp. 346-358.

13- Clarke, W.J., rt Micro fine Cement Techn%gy", 23rd International Cement Seminar, Atlanta, Georgia, December 6-9, 1987.

14- Zebovitz, S., Krizek, R.J., Atmatzidis, O.K., "Injection of Fine Sands with Very Fine Cement Grout", Journal of Geotechnical Engineering, Vol. 115, No 12, Dec. 1989, pp. 1717-1733.

15- Saleh, K., Mirza, J., Ballivy, G., MOlf, T., "Selection criteria for Portland and microfine Cement-based injection grouts", International Conference on Grouting in Rock and Concrete, Salzburg, Autriche, Oct. 1993.

16- Schwartz, L.G., Krizek, R.J., "Effects of mixing on rheological properlles of microfine cement grout", Proceeding Conference on Grouting, SOli Improvement and Geotech., ASCE, New Orleans, La., 1992, pp. 512-525.

17-Lea, F.M., "The chemistry of cement and concrete", Chemical publishmg company Ine., third edition, 1971, 727 pp .

18- Shimoda, M., Ohmori, H., "Ultra fine grouting materia/", Proceeding Conference on Grouting in Geotech., ASCE, New Orleans, La., 1982, pp. 77-91.

19- Tsivilis, S., Tsimas, S., Benetatou, A., Haniotakis, E., "Study on the contribution of the fineness on cement s treng th " , Zement-Kalk-Gips, Vol 43, No 1, 1990, pp. 26-29.

20- Derucher, K.N., Korfiatis, G.P., "Materials for civil and highway engineers", Second edition, Prentice Hall, 1988, 514 pp.

21- Fiorato, A.E., Burg, R.G., "Engineering properties and testing of High­Strength Concrete", Proceedmgs 1993 CPCA/CSCE Structural concrete conference, Toronto, May 19-21, 1993, pp. 322-329.

22- Canadian Portland Cement Association, "Design and Control of Con cre te Mixtures", Fourth edition, 1984, 151 pp.

23- Mehta, P.K., "Concrete: structure, properties and materia/s", Prentice-Hall Inc., 1986, 450 pp .

156

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24- Double, 0.0., "New developments in understanding the chemistry of cement hydration", Proceedings of a Royal Society Discussion Meeting - Technology in the 1990s: Developments in hydraulic cements, London, 1983, pp. 53-66.

25- Rlxom, M.R., Mailvaganam, N.P. "Chemical admixtures for eoncrete", E. & F.N. SPON, Second edition, , 1986, 306 pp.

26- Houlsby, A.C., "Cement grouting: water minimising practises.", Issues in Dam grouting, ASCE, Denver, 1985., pp. 34-75.

27-ASCE Grouting Cirnmittee (1980), "Pre/iminary .g/ossary of ter ms to grouting", ASCE Journal of geotechnical Division, Vol. 106, pp. 803-815.

28- Gerhart, P.M., Gross, R., "Fundamenta/s of fluid mechanics" , Edition Addison Wesley, 1985, 856 pp.

29- Ritchie, A.G.B., "The rheology of cement grout" , Cement and Lime Manufacture, January 1965, pp. 9-17.

30- Brookfield engineering laboratories, "More solutions to sticky problems: a guide to getting more from your Brookfield viscometer"

31-Clarke, W.J., Boyd, M.D., Helai, M., "U/trafine Cement Tests and Dril/ing Warm Springs Dam", ASCE, 1993.

32- Deere, D.U. et Lombardi, G. "Grout slurries - thick or thin?", Issues in Dam Grouting, ACSE, Denver, ~985, pp. 156-164.

33- Vorn Berg, W., "Influence of specifie surface and concentration of solids upon the flow behaviour of cement pastes", Magazine of concrete research, Vol. 31, No. 109,1979, pp. 221-216.

34- Ballivy, G., Saleh, K., Mnif, T., Baalbakl, M., "Note technique sur les essais de caractérisation et l'utilisation des coulis de ciment", Deuxième colloque sur la consolidation et la réfection des infrastructures par les techniques d'injection, Université de Sherbrooke, May 1992, pp. 283-297.

35- Ballivy, G., Saleh, K., Mnif, T., Mirza J., Rivest, M., "Coulis de ciment pour injection de micro fissures" , 2ième COlloque canadien sur le ciment et le béton, Vancouver, Canada, June 1991, pp. 291-300 .

157

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36- American Society for Testing and materials ASTM 0 2845-83, "Annual book of ASTM standards", vol. 04.08, Soil and Rock, building stones, geotextiles, 1986, pp. 317-321.

37- Daoud, M., Ballivy, G., "Essai ultrasonique-cahier no 5", Laboratoire de Mécanique des roches, Université de Sherbrooke, 1992.

38- Mnif, T., "Contribution à l'étude des caractéristiques mécaniques et physiques des coulis d'injection à base de suspensions de ciment", Master thesis, Sherbrooke University, 1993.

158

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APPENDIX A

VISCOSITY CALIBRATION CURVES

A-I

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:> N

• e -Calibration curves - Spindle 1

500" ----~----------------------------------

Ci) 400 a. o '-'

~ ~ 300 en o o en .-~ 200 .> 1\1 -Cl> a: 100·· .. ~ ..

o 500 1000 1500 2000 Viscosity read (apparent) (cps)

Angular speed

-0- 60 RPM

+30 RPM

~ 12 RPM

-6 RPM

*3 RPM

2500 3000

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> 1 W

--------------------------------..... • • • Calibration curves - Spindle no 2

500,

Ci) 400 r - - - - -u -/'- - --a. ......... ~ ~ 300 en o o en .-

: - - - - - - - - - - : - - - - - /- - - ; - - . - - - . - .. ; . - -

~ 200 >

- - - - - -. - - . ;,'- . - - -. - - - - - - - - - . Angular speed

.-âi -Q)

a: 100

o 500

-0- 60 RPM

+30 RPM

- - - - • - • • • - - - - - - • - 1 * 12 RPM

--6RPM

~3 RPM

1000 1500 2000 2500

Viscosity read (apparent) (cps) 3000

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> J,..

• • • Calibration curves - Spindle no 3

5001r-------------------------------------~

u; 400 · ........ . c- ., ~ o -~ ~ 300 CI)

o o CI)

.~ 200 > ca -ID CI: 100

o 500 1000 1500

_.~--- ----------

Angular speed

--- 50 RPM

-:- 30 RPM

* 12 RPM

-SRPM

*3 RPM

2000 2500 3000

Viscosity read (apparent) (cps)

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> , v.

• • • Calibration curves - Spindle no 4

500,1 ----~--------------------------~

en 400 r - - - - - -

a. u . U·

-~

:: 300 en o o (J) .-~ 200 > ca -Q)

a: 100

o

~ - - - - - - -/ ' 1 - - • ~ - • '/ - - . -, -

-~---._--._-~-- ..

~ , ,

500 1000 1500 2000

Viscosity read (apparent) (cps)

Angular speed

-0- SO RPM

+30 RPM

* 12 RPM

--SRPM

*3 RPM

2500 3000

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APPENDIX B

VISCOSITV TABLES

B-l

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Cj 1

N

• • Table 8-1 Relative viscosities (just after mixing) vs. initial w/e ratios at 4 oe, 100 e and 200 e

Imtial W/C 04 0.5 0.6 Temperature 4 10 20 4 10 20 4 10

(OCl Type . 278 264 158 . 152 105 110

10

C Type > > > 352 288 211 298 230 30 750 750 750

E Mlcrocem --- --- --- 515 518 · 375 382 650SR

M Mlcrocem > > > · 582 574 313 293

900 750 750 750

E Lenka 99 --- 85 84 --- · 21 ---737

N Sponor --- --- --- > > > > > A16 1000 1000 1000 750 750

T Sponor --- --- --- --- --- 105 --- ---A 16 +spl

S MC --- --- --- · --- --- . ---500 MC --- --- --- > > > > >

500+SP 1000 1000 1000 750 750

Sponor --- --- --- > > > > > A12 1000 1000 1000 750 750

Spmor --- --- --- --- --- 50 --- ---A12+Spl

Spmor --- --- --- --- --- 25 --- ---A12+Sp2

Spmor --- --- --- · . · > > E12 1000 1000

Sponor --- --- --- > > > --- ---E12+Spl 1000 1000 1000

---: Not performed * : Va~ue not accurate 1 : 1.2% (dry weight) of SP by cement weight 2 : 4.0% (dry welght) of SP by cement weight

Relative viscosltv (cps) 0.8 1.0 1.2

20 4 10 20 4 10 20 4 10 20

100 41 39 36 18 19 19 10 10 11

136 113 105 103 68 47 37 21 21 20

350 250 211 137 90 . 93 . . 50

303 121 120 117 65 68 62 29 . . 27 5 --- 12 3 --- 6 2 --- . > 386 415 400 221 225 222 110 121 100

750

--- --- --- 43 --- --- --- --- --- 2

--- 416 --- --- 262 --- --- 128 --- ---

> 313 282 300 153 175 193 88 90 71 750

> 388 398 400 294 . 275 . 120 108 750

--- --- --- 6 --- --- --- --- --- 2

--- --- --- 3 --- --- --- --- --- 2

> > > > 396 338 . 262 258 288 1000 750 750 750

--- --- --- 307 --- --- --- --- --- 25

1.5 2.0 4 10 20 4 10 20

6 6 5 3 3 3

11 11 13 6 6 5

31 26 20 11 11 11

16 17 17 8 9 9

2 --- 2 2 --- ---

60 58 67 33 22 21

--- --- --- --- 1

94 -- --- 44 --- ---

71 59 38 --- 13 15 1

51 52 . 26 23 25

--- --- --- --- 1

--- --- --- --- --- 1

. 117 115 68 63 60

--- --- --- --- --- 8

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t:p '-'

• • Table 8-2 Relative viscosities (at 60 minutes) vs. initial W le ratio at 40C, 100C and 200C

Initiai W/C 0.4 0.5 0.6 Temperature 4 10 20 4 10 20 4 10

(OC)

Type 276 315 263 200 187 219 116 120 10

C Type > > > 447 380 243 · 253 30 750 750 750

E Mlcrocem --- --- --- 523 . . · 467 6S0SR

M Mlcrocem > > > > > > · 407 900 750 750 750 750 750 750

E lanko 98 --- 88 90 --- --- 38 ---737

N Spmor --- --- --- > > > 482 . A16 1000 1000 1000

T Spmor --- --- --- --- --- 110 --- ---A16+SP'

S MC --- --- --- --- --- --- --- --500 MC --- --- --- > > -. > >

SOO+SP 1000 iVOO 1000 750 750

Spmor --- --- --- > > > > > A12 1000 1000 1000 750 750

Spmor --- --- --- --- --- 62 --- ---A 12 +SP'

Splnor --- --- --- --- --- 26 --- ---A 12 +S.,2

Spmor --- --- --- . . > > E12 1000 1000

Spmor -- --- --- --- - - > --- ---E12+SP' 750

---- -------: Not performed • : Value not accurate 1 : 1.2% (dry weight) of SP by cement weight 2 : 4.0% (dry weight) of SP by cement weight

Relative viscositv (cps) 0.8 1.0 1.2

20 4 10 20 4 10 20 4 10

214 50 53 100 23 25 22 13 14

· 123 123 110 75 61 57 28 27

· 251 207 177 103 161 130 99 101

402 133 153 . 96 79 99 37 35

29 . --- 14 9 --- 7 8 ---

· . 429 536 236 291 222 125 162

--- --- --- 7 --- --- --- --- ---

--- --- --- --- --- --- --- --- ---

> 508 414 292 268 224 141 161 132 750

> 371 502 550 301 318 310 188 201 750

--- --- --- 43 --- --- --- --- ---

--- --- --- 43 --- --- --- --- ---

> > > > 383 381 539 281 249 1000 750 750 750

--- --- --- 325 --- --- --- --- ---

1.5 2.0 20 4 10 20 4 10 20

12 7 7 6 4 4 3

29 13 15 16 7 7 7

80 78 45 40 18 18 16

. 14 15 26 9 7 9

--- 5 --- 4 3 --- ---

154 84 82 107 30 32 28

2 --- --- --- -- --- 1

--- --- --- --- --- --- ---

85 84 78 49 46 11 18

161 59 96 91 34 34 42

2 --- --- -- --- --- 1

2 --- --- -- --- --- 1

436 --- 164 252 72 98 lOS

27 --- --- - - --- --- 9

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APPENDIX C

SUSPENSION VOLUMES TABLES

Col

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(j 1

N

e • Table C-1 Volumes in suspension after 120 min vs. of initiai W/C ratios at 40C, 100C and 200C

W/C ratio 0.4 0.5 0.6 Temperature 4 10 20 4 10 20 4 10

(OCI Type 98 98 99 96 96 98 92 92

10

(' Type 100 100 100 99 100 100 99 98 30

E Mlcrocem 100 100 100 100 100 100 100 100 650SR

M Mlcrocem 100 100 100 100 100 100 99 99 900

E Lanko 99 100 99 98 737

N Spmor 100 100 100 100 100 100 100 100 A16

T Spmor --- --- 100 --- --- 100 --- ---A16+Spl

S MC --- --- --- --- --- --- --- ---500

MC 100 100 100 100 100 100 100 100 500 +SP Spmor 100 100 100 100 100 100 100 100 A12

Splnor --- --- 100 --- --- 100 --- ---A 12 + SP'

Spmor --- --- 100 --- --- 100 --- ---A12 + Sp2

SPlnor 100 100 100 100 100 100 100 100 E12

Splnor ---1

-- 100 -- --- 100 --- ---E12-.-Spl

---: Not performed * : Value not accurate 1 : 1.2% (dry welght) of SP by cement weight 2 : 4.0% (dry welght) of SP by cement welght

Volume in suspension (%) 0.8 1.0 1.2

20 4 10 20 4 10 20 4 10 20 4

97 86 89 88 84 83 80 79 77 71 65

99 90 93 95 89 87 87 86 86 86 85

l 'lO 99 99 99 98 98 98 95 96 96 83

99 99 98 99 97 96 98 91 90 97 92

100 99 99 95 98 97 96

100 100 100 100 98 98 99 97 97 99 94

--- --- --- 96 --- --- --- --- --- 89 ---

--- --- --- --- --- --- --- --- --- --- ---

100 100 100 100 98 99 99 97 98 99 94

100 99 100 100 97 99 99 96 98 99 Sl6

--- --- -- 99 --- --- --- --- --- ~7 ---

--- --- --- 98 --- --- --- --- --- 98 ---

100 100 100 100 100 100 100 100 100 100 98

--- --- --- 100 --- --- --- --- --- --- ----

1.5 2.0 10 20 4 10

20 .

62 58 48 46 43 1

85 83 74 71 74 •

79 79 77 70 1

89 92 88 86 77 ,

93 92

97 98 87 89 95

-- - - --- --- 82

--- --- --- --- ---

95 97 91 93 90

95 98 83 94 93

-- -- -- --- 95

--- --- --- --- 98

99 99 96 96 99

- - --- --- --- 98

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('j 1 ~J

e

Table C-2 Final volumes in suspension vs. initiai W/C ratios at 40C, 100C and 200C

Volume in suspension (%) W/C ratio 004 05 0.6 08 1.0 Temperature 4 10 20 4 10 20 4 10 20 4 10 20 4 10 20 4

(OCI Type 9B 9B 99 95 95 97 85 B7 95 77 80 80 6B 68 71 62

10

C Type 100 100 100 99 100 97 99 98 95 90 89 88 85 81 81 76

30

E Mlcrocem 100 100 100 100 100 100 100 100 99 99 98 99 99 . 98 94 6S0SR

M Mlcrocem 100 100 100 100 100 100 99 99 99 99 98 99 97 95 98 90 900

E Lenko 99 000 100 99 00- __ 0 9B --- 99 99 _00 99 91 0-- 9B 54 737

N Splnor 100 100 100 100 100 100 100 100 100 100 100 100 97 98 99 97 AIS

T Splnor 0_- --- --- --- --- --- --- --- --- --- --- --- --- --- --- ---A16+Spl

S MC --- --- --- --- --- --- --- --- --- --- --- --- --- --- --- ---500 MC 100 100 100 100 100 100 100 100 100 100 100 100 98 99 99 97

500 +SP Splnor 100 100 100 100 100 100 100 100 100 99 100 100 97 99 99 95

A12 Spmor --- --- --- _0- --- --- --- --- --- --- --- --- --- --- -0- ---

A 12 + Spl Splnor --- --- --- --- --- --- --- --- --- --- --- --- --- --- --- ---

AI2+SP2

Spmor 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100 100

E12 Splnor --- --- --- --- --- _0- --- --- --- --- --- --- --- --- --- ---

E12+Spl - - "---- -- --

---: Not performed * : Value not accu rate 1 : 1.2% (dry welght) of SP by cement weight

2 : 4.0% (dry weight) of SP by cement weight

----

1.2 1.5 20 10 20 4 10 20 4 10 20

62 64 50 54 54 42 43 42

77 74 68 70 64 54 55 52

96 94 75 7B . 66 66 62

86 95 B3 83 . 78 78 . --- --- 79 --- --- 66 --- ---

96 . 90 96 98 82 86 . --- --- --- --- --- -- --

--- --- --- --- --- --- --- ---

98 99 94 94 97 86 84 85

97 99 94 93 98 91 92 93

--- --- --- - - _0- _0- --- __ 0

--- --- --- --- --- --- --- ---

100 100 98 99 99 96 96 99

--- --- --- --- --- --- --- ---

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APPENDIX 0

SETTING TIME TABLES

0-1

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o . N

• • Table 0-1 Initial setting time vs. initial W/C ratios at 40C, 100C and 200C

W/C ,atio 0.4 0.5 0.6 Temperature 4 10 20 4 10 20 4 10

(OC)

Type 155 11 3 60 183 143 77 230 146

10

C Tvpe 85 63 35 100 80 50 135 93 30

E Mlcrocem 50 55 55 113 93 60 135 107

650SR

M Mlcrocem 1 3 10 09 23 21 1 3 35 275 900

E Lanko 110 ... 58 145 ..- _.- lS 2 ---737

N Splnor .-- --- --- 93 60 43 135 80 A16

T Splnor ._- --- --- -_. -.- 80 --- ---.A16+SP1

S MC ... --- --- ._- --- -_. lla ---500 MC _ .. --- _.- 180 120 78 >24 178

500+SP

Splnor ._. --- --- 75 67 43 85 83

A12 Splnor --. -_. _.- 210 --- 88 --- ---

A12+SP'

Splr Jr , ... _. . _. --. ..- >24 --- _ .. A 12 + SP-

Splnor .. - --- --- 03 03 04 1 3 06 E12

Spmor . _. _ .. -_.

1

. .. 100 _ .. ._-E12+SP1

---: Not performed • : Value not accurate 1 : 1.2% (dry welght) of SP by cement weight 2 : 4.0% (dry welght) of SP by cement welght

Initial settin~ tiFIle (hours) 0.8 1.0

20 4 10 20 4 10 20

90 232 175 110 >24 >24 130

55 177 124 8.0 210 170 90

73 210 143 92 240 183 107

1 5 50 37 22 95 75 65

76 >24 --- 83 >24 --- 925

50 19 a 103 65 243 15 S 90

._- --- --- 140 --- --- ---

--- 218 --- --- >24 --- ._-

85 >24 >24 156 >24 >24 190

54 157 143 78 21 0 178 98

--- >24 .. - 108 .-- ._- ---

._- .. ._- >24 .. - ._. ._-

0'" 140 150 93 >24 190 135

--- ... --- 170 .. - --- ---

1.2 1.5 2.0 __ 4 10 20 4 10 20 4 10 20

>24 >24 170 >24 >24 >24 >24 >24 >24

>24 185 140 >24 >24 >24 >24 >24 >24

>24 203 129 >24 >24 >24 >24 >24 >241

>24 >24 >24 >24 >24 >24 >24 >24 >24

>24 -_. --- >24 .- 125 >24 ._. . ..

>24 183 "3 >24 >24 120 >24 >24 170

--- _.- ,gO ._ . ._- .. - . - _ .. >24

>24 --- --- >24 ... .. >24 -- .-

>24 >24 >24 >24 >24 >24 >24 >24 >24

>24 207 11 6 >24 >24 130 >24 >24 190

>24 --- 177 ... _ .. ... >24 .. >24

.. - ._- >24 --- .. ... . . .. > 24

>24 >24 158 >24 >24 180 >24 >24 240

--- _.- 190 --- _ .. ... _ .. .. >24

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1::7 • w

• e

Table 0-2 Final setting time vs. initial W IC ratios at 40C, 100C and 200e

!.W/C ratIo 0.4 0.5 0.6

1

1 1

.. emperature 4 10 20 4 10 20 4 10

(OC)

Type 178 140 73 203 186 98 >24 190 la

C Type 11 3 78 53 183 97 63 200 131 30

E Mlcrocom 95 80 70 14.3 11 1 78 173 140

650!;R

M Mlcrocem 1 8 ~5 1 1 3<: 38 16 38 45 !

900 ~

E Lar.ko 130 ... 75 168 .. ' --. 21 2 .--737

1'01 SOlnor --. . .. --- 133 76 50 165 90 AIS

T Splnor .-- _ .. --- --- --- 90 --- _.-A16+Sp1

S MC --- ... --- --- ..- --- 232 ---500 MC .. - --- --- >24 154 90 >24 195

500+SP

5plnor --- --- .-- 110 87 53 133 9&

A12 Splnor --- --- --- >24 --- 93 --- ---

A12+Sp t

Splnor A 12 + Sp2

--- --- --- --- --- >24 --- ...

Sp.nor --- _o. --- 22 08 1 0 63 43

E12

Splnor --- --- --- _o. .-- 108 ._- .. -E12+Sp1

---: Not performed * : Value not accurate 1 : 1 .2% (dry weight) of SP by ~ament weight 2 : 4.0% (dry weight) of SP by cement weight

Final settino time (hours) 0.8 1.0

20 4 10 20 4 10 20

130 >24 >24 160 >24 >24 175

77 225 166 103 240 230 115

93 >24 193 11 5 >24 253 147

20 98 98 58 142 130 100

88 >24 .-- 110 >24 --. 125

56 240 123 73 >24 235 140

--- --- .. - 160 ..- --- ---

--- >24 .. - --- >24 --. ---1

110 >24 >24 207 >24 >24 >24

65 170 178 93 >24 21 !: 148

--- >24 --- 130 --- --- ---

'-- '-- ... >24 -'- --- ---28 >24 178 120 >24 225 170

.. - ._- --- 190 .-- -" _o.

-- - 1.-..

e

1 2 1.5 20 4 10 20 4 10 20 4 la 20

>24 >24 >24 >24 >24 >24 >24 >24 >24

>24 >24 220 >24 >2 .. >24 >24 >24 >24

>24 >24 165 >24 >24 >24 >24 >..14 >24

>24 -,24 >24 >24 >24 >24 >24 >24 >24

>24 .-- ... >24 178 >24 --. ..

>24 >24 155 >24 >24 20 B >24 >24 >24

--. --- 230 -- --- --- --- _ .. >2<'

>24 --- --. >24 --- --- >24 ... ---

>24 >24 >24 >24 >24 >24 >24 >24 >24

>24 =-24 156 >24 >24 193 >24 >24 >24

>24 --- 220 _o. --- .-- >24 --. >24

-- --- >24 --- --- --- --- .. >24

>24 275 188 >24 >24 25 B >24 >24 >24

... --- 205 . -. --- --- --. --- >24

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APPENDIX E

MODUlUS OF ELASTICITY AND

POISSON'S RATIO TABLES

E-l

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[TI 1

N

- -Table E-1 Modulus of elasticlty vs. initiai W/C ratio at 40C, 100C and 200C

Modulus of elasticity (GPa) Instial W/C 0.4 0.5 0.6 0.8 1.0 Temperature 4 10 20 4 10 20 4 10 20 4 10 20 4 10 20

(OC)

Type 15 1 180 156 11 3 162 132 105 157 11 7 100 142 120 91 12 1 102

10

C Type 162 166 . 126 139 161 104 125 11 3 72 101 76 62 80 54 30

E lli'icrocem 185 180 177 122 148 14 ~ 98 108 98 65 60 59 39 63 43

6S0SR

M Mlcrocem 145 132 163 120 108 114 76 74 103 55 74 71 35 61 41

900

E Lanko 174 --- 133 122 --- --- 93 --- 11 7 64 --- &8 42 --- 46

737

N Splnor --- --- --- --- --- --- --- --- 115 --- --- 11 3 --- --- 66

A1S -T Splnor --- --- --- --- --- --- --- --- -- --- --- --- --- --- ---

A16+Spl

S MC --- --- .. - --- --- --. --. --- .-- --- --- --- --- --- ---500

MC --- --- --- --- --- 171 --- --- 15 1 --- --- Il 2 --- --- 97

"OO+SP Splnor --- --- --- --- --- 162 --- --- 152 --- --- 86 --- --- 75

A12

Splnor --- --- --- 123 --- --- 76 --- .. - 58 --- --- 46 --- ---E12

Splnor --- --- --- --- --- --- --- --- --- --- --- --- --- --- ---E12+Spl

---: Not performed *' : Value not accurate 1 : 1.2% (dry weight) of SP by cement weight

~ 1

1.2 1.5 2.0 4 10 20 4 10 20 4 10 20

73 93 90 50 72 77 . 65 61

48 60 54 55 50 62 41 47 ---

25 24 39 22 24 • 38 19 - - 33

31 26 30 29 25 25 --- --- 1 3

45 --- --- 39 --- 41 30 --- ---

--- --- 48 --- --- -- --- --- ------ --- --- --- --- --- --- --- ---

--- --- --- --- --- --- -- --- ---1

--- --- 63 --- --- 58 --- --- ---

--- --- --- --- --- 58 --- --- 40

29 --- --- 1 9 --- --- 07 --- ---

--- --- --- --- --- --- --- --- --

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• • • Table E-2 Poisson's ratio vs. w/e ratio at 4oe, 100e and 200 e

Initiai W/C 2.0 Temperature 10 1 20

(OCI T'/pe 011 01610121012101410131012! 0141 013

10

C [ Type 014 0171016101310161016101210141015 30

E 1 Mlcrocem 01<; 017 1015 1 C 16 1 013 1 014 1017 1 012 1015 650SR

M Mlcro('em 011 1014 1 1 011 1 ._- 1 --- 1 015 900

E Lanko 013 1 --- 1 1 012 737

N Spmor 1 --- 1 1 --- 1 1 --- 1 --- 1 --- 1011 tn • A16 w

T Spmor A 16 + SP

S MC 500 MC 1010

500+SP Spmor 1010 1 1 011 A12

Spmor 1 010 1 1 010 E12

Spmor E12+SP

Not performed ... : Value not accurate 1 : 1.2% (dry weight) of SP by cement weight

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APPENDIX F

COMPRESSIVE STREf~GTH TABLES

F-l

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• • • Table F-1 Compressive strength vs. initial W/C ratio at 40C, 100C and 200C

fr.' (MPa) 1

1

Initial W/C 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Temperature 4 10 20 4 10 20 4 10 20 4 10 ~o 4 10 20 4 10 :~ 4 la 20 4 la 20

(OC)

Type 480 620 654 318 520 455 286 390 314 . 307 167 140 247 149 11 7 240 120 93 149 95 69 18 '"7"2 10

C Type 591 687 . 442 682 684 278 . 362 180 210 221 108 15 1 127 104 128 81 83 99 . 1 81 87 63 30

E M.eroeem 625 579 768 546 574 608 339 400 386 165 20 8 173 la 6 165 la 1 59 57 64 35 48 60 29 20 39 650SR

M Mlcrocem 555 . 620 498 602 397 285 426 325 146 19.1 21 1 80 11 4 105 61 57 58 55 45 35 32 . 15 900

E Lanko 737 574 --- 680 476 --- --- 377 --- 480 206 --- 271 102 --- 139 93 --- --- so --- la 3 39 --- ---

'TJ , N Splnor 0_- 000 _00 00-

__ 0

00- 00

__ 0

406 _0- _00 280 000 _00 136 00- 000 119 00- _0 53 00 -00 42

A16 • N

T Splnor _0- 0_- --- --- __ 0 --- --- 0_-

__ 0

0_0 0_-

__ 0 --- --- --- -0- --- 0_- 0-0 --- --- --- --- ---A 16 + SpI -

S MC -00 _0- 0_0 000 000 000 000 --0 0-- --0 00 -00 _0- 00- 000 000 _00 --- --0 --- 0- _-0 -- ---500

1

MC 000 --- --- 0_0 _0- 393 _00 --- 342 000 000 :'0 8 000 0_- 127 _0- _00 121 0_- 00- --- --- --- ---500 +SP

Splnor -0- 0_- --0 0_- 0_- 303 0-- -00 169 000 0_- ~ 1 0 000 , --0 95 00- 0_0 .

--0 --- 89 000 000 81

A12

Splnor 0_- --- -00 372 _0- 268 333 --. 204 255 _00 170 168 000 167 96 00- 100 62 0-0 32 15 --0 13

E12 Splnor --- 00- --- --0 --- --- --- --- --- --- --- --- 0_0

__ 0 --- 000 000 --0

__ 0 -00 00 --- 000 00-

E12 +Spl - - _. - -- L- ..

---: Not performed .. : Value not accu rate 1 : 1.2% (dry welght) of SP by cement weigl"lt

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• APPENDIX G

BOND STRENGTH (TENSILE) TABLES

• G-l

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• • -t

Table G-1 Bond strength (tensile) vs. initial W/C ratio at 40 C, 100 C and 200 C

Initial W/C 2.0 Temperature 1 10 1 20

(OC)

Type

24

1 11041°181 1 089

10 1 00 1 024 C 041 1 15 028

E 032 1 1 106 1 022

M 031 1 1 068 900

E lanka l , 28 1 1 1 32 1 075 1 1 083 737

0 N Sponor 1 --- 1 1 --- 1 Ù 42 1 1 080 1 039 1 --- 1 033 IV

A16

T Splnor A 16 + SP 1

S MC 500

MC 1 049 1 1 1 28 1011 1 1 067

SOO+SP Sponor 1 049 1 1 1 01 1 036 1 1 086 Al?

Spmor --\

-- 1 071 1 \, 20 1 060 1 1 097\ 054 1 E12

Sp.nor E12+Spl

Not performed

* : Value not accurate 1 : 1.2% (dry welght) of SP by cement welght

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APPENDIX H

UL TRASONIC PULSE VELOCITIES AND

DYNAMIC ElASTIC CONSTANTS

H-I

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• • • Table H-' Conlpression wave velocity (Vp) vs. initial W/C ratios 8t 40C, 100C and 200C

Compression wave velocity (mIs) Initial W/C 0.4 0.5 0.6 0.8 1.0 1.2 1 5 2.0 Temperature 4 10 20 4 10 20 4 10 20 4 10 20 4 10 20 4 10 20 4 1 10 20 4 10 20

(oCI

Type 3230 3747 3216 3055 3574 3175 2870 . 3000 2700 3259 2765 2495 3031 2645 2280 29ïl 2470 2030 . nE5 1700 · 2075

10

C Type 3461 3752 . 3276 3466 3406 2975 . 2940 255'" 2832 2692 2350 2730 2524 2265 2558 2560 2115 2454 2348 1905 2226 2190

30

E Mlcrocem 3465 3454 3469 310ü 3311 3195 2805 296') 2930 2272 2391 2504 1981 2454 2263 1643 1696 2141 1488 1429 2060 1455 · 1952

650SR

M Mlcro:::em . . 3465 3430 3512 3200 3155 3089 2871 2810 2392 2530 2000 . 2160 1840 1674 1860 1189 1521 . 1515 · . 900

E Lanko 3419 ... 3690 3570 000 000 2855 000 3914 2441 000 2533 2100 000 2096 1986 '00 000 1855 00 2492

737

N Splnor 000 00 000 '00 000 .00 o •• ..0 3078 0'0 0'0 3041 000 000 2813 .. , 000 2697 00 000 2597 2637

Al6 ::x: . IV

T Spmor 000 000 00' 000 000 00.

__ 0 _.- .-0 .. - --0 _0- 00' _0- 0-0 ... 000 0_0 000 000 00 00 00

A16+Spl

S MC 000 000 000 _00 000 ... ._. ,'0 000 o. 0'0 0.0 00' 000 000 00- .0. 00

500 MC 000 0_0 000 000 000 _0- 0_0 ... 3281 --. o •• 3011 . .. . .. 2578 ... ... "0 00' 0.0 2382 000

. 500 +SP

Spmor _'0 00- 00. .0. '0- 3407 00. . .. 3130 "0 00- .. - '0' ... . .. __ 0 000 •• 0 0_' _o • 2427 2333

Al2 Spmor 0_0 _00 3024 000 3524 2806 00-

. 2366 000 2429 2200 _0- 2203 1987 000 20B8 000 1492 lC50

E12

Spmor 00 000 0_0 000 0.0 o •• .,. 000 00- 00' 0.0 00- • 00 ... o.' 00 000 000 00

E.2.Spl

---: Not performed .. : Value not accurate 1 : 1.2% (dry welghtl of SP by cement weig:--t

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• • • Table H-2 Shear wave velocity (Vs) vs. initial W/C ratios at 40C, 100C and 200C

Shear wave veloclty (m/s) InitiaI W/C 04 05 0.6 08 1 0 1 2 1 5 20 Temperature 4 10 20 4 10 20 4 10 20 4 10 20 4 10 20 4 10 20 4 10 20 4 10 20 (OC)

Type 1977 2070 2000 1844 1926 1900 1761 . 1789 1631 1845 1584 1545 1758 . 1459 1587 1770 1318 . . 1203 . · 10

C Type 2150 2058 . 2020 2020 1983 1822 . 1787 1546 . 1543 1454 1532 1401 1380 1453 1386 1280 1351 1327 1223 1225 11'1.0 30

E Mlcrocem 2192 1992 . 1958 1870 1887 1800 1685 1760 1400 1476 1576 1147 . 1837 977 1009 1700 899 869 863 837 1258 6S0SR

M Mlcrocem . . 2232 2241 1938 2125 184b 1862 1796 1622 1475 1650 1212 . 1342 1149 987 1226 1073 889 . 935 . · 900

E Lanko 737 2041 --- --- 2210 --- --- 1786 --- 2149 1310 --- 1451 1201 --- 1229 1155 --- --- 1062 1100 . -- --f- .

N Spmor --- --- --- --- --- --- - - --- 1827 --- --- 1711 --- --- 1612 --- --- 1547 --- 1472 1417

::= '-'

A16 -T Sp.nor --- --- --- --- --- --- --- --- --- --- --- --- --- --- --- --- --- --- --

A16+Sp'

S MC --- --- -- --- --- -- --- --- --- --- --- --- --- --- --- ._. --- --- --- --

500 MC -_. ... ._- ._- .. - ._ . --- -_. 1694 ... --- 1811 ._- ._- 1523 .. ' -.' . ._. - - 1351 -- ·

500+SP

Spmor . " -_. ._- --- -_. 1940 ._. ._ . 1885 ._- __ a . __ a __ a

1471 __ a __ a . .-. --- 1365 1315

A12 Sp'Clor __ a __ a __ a 1842 __ a 2006 1648 ... . 1518 __ a 1464 1150 ". 1318 988 __ a 1293 . ._. 901 -_. --- 654

E12

Spmor .-. ._. --- --- --- __ a --- __ a __ a -_. ._. __ a _.- __ a __ a __ a __ a .-- _.- --- --- -- _.-E12+Sp1

---: Not performed * : Value not accu rate 1 : 1.2% (dry weight) of SP by cement weight

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::I: .!..

• -Table H-3 Dynamlc modulus of elasticity (Ed) vs. initiai W/C ratios at 40C, 100C and 200C

Dynamic modulus of elasticit~ (MPa) Initiai W/C 04 05 06 0.8 1.0 1.2 Temperature 4 10 20 4 10 20 4 10 20 4 10 20 4 10 20 4 10

(OC)

Type 188 246 195 162 225 176 139 · 151 116 173 11 7 99 145 105 87 125 10

C Type 223 253 . 187 228 184 144 · 141 96 192 104 77 17 2 84 71 143

30

E M,crocem 229 249 183 168 226 167 133 21 1 138 7B lB 6 97 50 '8 ::i . 32 163 650SR

M Mlcrocem . . 209 21 8 . 189 144 · 137 110 . 105 5 , . 60 42 . 900

E lanko 206 .. 239 21 8 ... ." 136 ... 21 0 72 . .. 192 57 . .. 162 54 . ..

737

N Sp,nor ... . " ... . .. . . ." ... . .. 201 ... . .. 200 '.' . .. 182 . .. . . A16

T Sp,nor ... ... . .. . .. . .. . .. . .. ... . .. . .. . .. . .. . .. . .. . .. . .. .. ' A 16+SP

1

S MC ... ... . .. ... . .. ... . .. . .. ... ... . .. . .. .-- . .. --. --. '--500

MC ... --' -- . '-- ... --' ... --. 21 4 . " --. 200 --. ... 182 ... .. '

500 +SP Sponor ... . -- --. --. .-- 21 7 .. . --. 20 S . -- ... . .. . .. . " 166 ... ...

A12

Spmor 156 233 102 . 84 --. 192 49 --' 173 35 --. -- '-- --. -- --. E12

Sponor . . . -- ... .-- ... .-- ... . .. '-- --' --' --. --. . . --. . .. . ..

E12 ... SP' ._.

Not performed + : Value not accurate 1 1.2% (dry welght) of SP by cement welght

e

1.5 20 20 4 10 20 4 10 20

i 110 64 . 84 45 . 66

82 59 122 73 49 94 54

58 25 13 B 60 2 5 113 56

51 41 . . 27 . . . '. 43 . .. 130 . .. . .

175 ... ... 161 141

". . .. . .. ..

'-- --. . .. --

175 ... 161 .. 141

... --. . .. 166 .. .. 147

164 . 159 . 144

.-- ... .-- --. --.

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:I: • Ut

• • Tab'e H-4 Dynamic Poissol '("~ ratio (vd) vs. initial W/C ratios at 40C, 100C and 200C

Poisson's ratio Initiai W/C 0.4 0.5 0.6 0.8 1.0 Temperature 4 10 20 4 10 20 4 10 20 4 10 20 4 10 20 4

(OC)

Type 017 028 019 018 030 022 015 . 024 020 026 026 025 024 025 023 10

C Type 019 028 . 020 024 024 020 . 021 021 031 026 023 027 028 o 21 30

1 Mlcrocem 017 025 029 018 027 023 015 026 022 020 019 017 025 021 . 023

650SR

M M,crocem 019 ... 022 013 ... 011 024 . .. 018 021 . .. 013 018 ... 022 017 900

E lanko 737 023 00' 026 019 '0' ... 019 ... 028 030 ... 026 025 '00 024 028

N Spmor o •• 000 "0 .0. 000 o" 000 00. 023 .00 0'0 027 o •• 0.0 026 o ••

A16

T Sprnor • 0. 00. 0'0 •• 0 ... 000 000 000 000 0.0 000 '00 000 000 000 '00

A16+SP'

S MC 0.0 000 0.0 0.0 .00 000 000 000 o •• o" .00 0.0 000 000 '00 •• 0

500 MC 000 000 000 00' "0 000 00' .00 022 '00 00' 022 '00 ... 023 0.0

500+SP Sprnor 000 00. 000

. .00 026 000 000 022 000 "0

. 00' 000 020 ...

A12 Sprnor •• 0 o" 0.0 023 000 026 024 .00

. 020 .00 021 027 000 022 030 E12

Sprnor 000 .00 .00 00. ... 0.0 ..0 .. 0 ... '0. ..0 .. 0 o.' ... . .. . .. E12+SP' .. _.

---: Not performed * : Value not accu rate 1 : 1.2% (dry weight) of SP by cement weight

1.2 1.5 2.0 10 20 4 10 20 4 10 20

030 . 021 ... 020 022 . 021

026 027 020 028 027 015 028 032

023 . 021 021 024 022 024 014

. .. 012 022 020 00 .

o •• 0.0 026 029 . . . o ••

"0 025 "0 .. 026 030

o •• '0 • 00. o • ." 00 000 00'

00' 00. 0'0 ... . .. ...

000 022 '00 00. 026 ... o' .

0.0 .

00. •• 0 027 ... 000 028

0.0 019 •• 0 ... 021 • 0' ... 018

•• 0 0.0 0" '0 ... . .. ... ...

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APPENDIX 1

VISCOSITY RESUL TS

1-1

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• 500

- Type 10 tJ) a. 400 0 -~ .U) 300 8 tJ)

'S; 200 CI) > ~ cu 100 CI)

œ:

\ \. ~

0 ~ . . . . o 0.5 1 1.5 2

Initial W/C ratio

1--4°C *" 10°C -â- 20°C 1

Fig. 1-' Relative viscosity of Type 10 cement at 0 min

• 500 Type 10

(i) 400 a. 0 -~

.U) 300 8 tJ)

'S; 200 CI) > ~ cu Q) 100 œ:

o~++++~~~~~~~~~~

o 0.5 1 1.5 2 Initial W/C ratio

• Fig. 1-2 Relative viscosity of Type 10 cement at 60 min

1-2

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• 500 Type 30 -'" 400 Q.

(J -~ 'iii 300 0 (J

'" '> 200 Cl) > :e:::o tU Q) 100 a::

0

0 0.5 1 1.5 2 Initial W/C ratio

1_4°C *" 10°C ~20°C

Fig. 1-3 Relative viscosity of Type 30 cement at 0 min

• 500 Type 30

-'" 400 Q. (J -~ 300 8 '" '> 200 Cl) >

:e:::o tU 'ëi) 100 a:::

0

0 0.5 1 1.5 2 Initial W/C ratio

1--4°C *10°C ~20°C

• Fig. 1-4 Relative viscosity of Type 30 cement at 60 min

1-3

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500 650SR

-'tn 400 Q. 0 -~ 'in 300 0 0 tn '> 200 Q) > :tJ ns Q) 100 a::

O+-~~~~~~~~~+-~~~~+-~~

o 0.5 1 1.5 2 Initial W/C ratio

Fig. '-5 Relative viscosity of Microcem 650SR cement at 0 min

500~------~--------------------~ 650SR

-~ 400+---------~----------------------~ o -~ '0 300+----------+~------------------~ 8 (h

'S; 200 +------~~--------"""'i Q) >

+=0 cu œ 100+---------~~~~-----~ 0::

o 0.5 1 1.5 2 Initial W/C ratio

Fig. 1-6 Relative viscosity of Microcem 650SR cement at 60 min

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500--------------------------------900 -~ 400 +---------------------------------~

~ ~ cn 300 +---------3----------------~ 8 fi) 'S 200 +-_____ "-_________ ---.1

~ .. tU ~ 100+---------~--------------~ ex:

o 0.5 1 1.5 2 Initial W/C ratio

Fig. '-7 Relative viscosity of Microcem 900 cement at 0 min

500 -r------------------. 900 -o 400 +----------~---------------------~ a. o -b

"Cn 300 -1------4\-------------1 8 o '5 200 -+-______ ~~-------------~ CI) > ~ al CI) 1 00 +-------~~._.oIIr__------I

ex::

o 0.5 1 1.5 2 Initial W/C ratio

Fig. 1-8 Relative viscosity of Microcem 900 cement at 60 min

1-5

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500

-CIJ 400 c. o -~ fn 300 8 tJ)

'> 200 ~ ~ tU Q) 100 0:

o

Lanko 737

--

'-• ....

o 0.5 1 1.5 Initial WlC ratio

Fig. 1-9 Relative viscosity of Lanko 737 cement at 0 min

500 Lanko 737

-fi) 400 a. 0 -~ fn 300 0 0 fi)

'> 200 Q) >

+=' cu Q) 100

ct:: ~ . . . . . o o 0.5 1 1.5

Initial W/C ratio

Fig. 1-10 Relative viscosity of Lanko 737 cement at 60 min

1-6

2

2

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• 500

1 MC500+SP

-fi) 400 0-0 -~ 'u; 300 0 0 fi)

'S; 200 Q) >

+=i cu ëi) 100 ct::

0 1 1 1 1

0 0,5 1 1,5 2 Initial W/C ratio

1 ... 4°C *10°C .20°C 1

Fig. 1-11 Relative viscosity of MC500 + SP cement at 0 min

• 500 MC500+SP

-tn 400 0-0 -~ 'u; 300 0 0 tn 'S; 200 Q) > :..:; cu Q) 100

ct::

0 + 0 0,5 1 1.5 2

Initial W/C ratio 1 ... 4°C *10°C *20o~

• Fig. 1-12 Relative viscosity of MC500 + SP cement at 60

1-7

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500 A12

- 400 fi) 0-0 ---~

'u) 300 8 fi)

'> 200 Q) > :.;:::; tU Q) 100 a::

o 0,5 1 1.5 2 Initial W/C ratio

Fig. 1-13 Relative viscosity of Spinor A 12 cement at 0 min

500~-----------n----------------~

-fi) 400+------------------------~~--------------------~ 0-o ---~ 'u) 300 +---------...... 11----------4 8 fi)

'~ 200 +----------------~WIi-------__t > :.;:::; tU Q) 100+-----------------------------~~~------~ a::

O+-~~+_~~+_f~~+_f~~~~~~~~~

o 0,5 1 1.5 2 Initial W/C ratio

Fig. 1-14 Relative viscosity of Spinor A 12 cement at 60 min

1-8

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500 -r------------------A16 -o 400 +-------------~------------------~ a. u -

~ "in 300 +-______ ---l~--------_' 8 o

.S; 200 +-________ ----:~-------_' ~ ;; co Q) 100 +------------------ -.~-----~ cr::

o ~~~~~~~-+~~~~~~+-~~~ o 0.5 1 1.5 2

Initial W/C ratio

Fig. 1-15 Relative viscosity of Spinor A 16 cement at 0 min

500 ,.......--------,------------.

-o 400 +-------~~------------~ a. u -~ "in 300 +-------------~k,.._---------___1 8 fn

.> 200 +-----------..:~..------~ ~

10 Q) 1 00 +-----------------~~..ao....,..__--~ cr::

o 0.5 1 1.5 2 Initial W/C ratio

Fig. 1-16 Relative viscosity of Spinor A16 cement at 60 min

1-9

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500--------------------------------~ E12 -~ 400+---------------__ ----------------~ C-

u .... --~ ën 300 +-----------------~r_::__----------~ 8 .!a > 200+---------------------~~--------~ Cl) > ~ cu Cl) 1 00 +------------------------=;:..,~-~~

cr:

o 0.5 1 1.5 2 Initial W/C ratio

Fig. 1-17 Relative viscosity of Spinor E12 cement at 0 min

500------------------~------------~ E12

o 400+-------------------~----------~ c-o -~ '0 300+-----------------~~--~--------~ 8 fi)

'> 200 +---------------------~~~~--~ CI) > ~ cu CI) 100+----------------------~---------~~ cr:

o 0.5 1 1.5 2 Initial W/C ratio

Fig. 1-18 Relative viscosity of Spinor E12 cement at 60 min

1-10

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• APPENDIX J

VOLUMES IN SUSPENSION RESUL TS

• }-1

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10 100 .....-----=---------.. ---:..!----.

-~ 80 -Q)

E ~ 60 > c: .~ 40 c: Q) ~ (/) 20 :::l

Cf)

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. J-l Sta bility of Type 10 cement after 1 20 min .

100 Type 10

-?J. 80 -Q)

E :::l 60 0 > c: 0 40 "in c: Q) ~ 20 (/) :::l en

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. J-2 Final stability of Type 10 cement

J-2

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100

-~ 0 - 80 cv E :::l 60 0 > c .Q 40 fIJ C cv c.

20 fIJ :::l

en

0

Type 30 -~ ,. ~

1 /

1- " f0- i-- -- - i-- -" .... /, ,

"" ;

1- - - -- 1--- i-- - ..--,

: , ~ ,

1- - - 1-- - - - 1--

" " J

i-; - - - --i - - -

, ;

: ..J.

, ..J. ..J. ..J. 4- ..J. . •

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. J-3 Stability of Type 30 cement after 120 min .

100

--'#. 80 -Q)

E :::l 60 0 > c .Q 40 fIJ C cv a. 20 fIJ :::l en

0

Type 30

- ... 1..

.~ ..

1 - ~ - 1..-

) ~ r;';'

~ - f-- 1-- 1-- ~ it-fi

1'"

f- ~ i-- ..-- 1-- 1-- ...... ....--

li, ~ f- i-- - 1--

I~ - -

1;, l'{ 1; I~

..J. + ..J. • T

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. J-4 Final stability of Type 30 cement

J-3

1

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-~ 0 -CI)

E :::1 ë > c 0 ·in c CI) a. fi) :::1 en

100

80

60

40

20

650SR

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. J-5 Stability of Microcem 650SR cement after 120 min .

100

-tf!. - 80 CI)

E ::::J 60 "'0 > c 0 40 .c;; c CI) a. 20 fi) :::1 en

0

650SR _r-- ...

- r-- ~ - ~ -

....

....

.....

~ ~

1-- 1-- - -1-- 1-- ~ 1-- ~ r-- - ~ 1-- 1--

4- 4- 4- • 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. J-6 Final stability of Microcem 650SR cement

J-4

~

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• 100 900 r-I-

- ~ ~ 80 ~

, ~ 1-- ~ 1-- 1-- ~ -CI) "

E :J 60 ,

~ ~ 1-- ~ ~ !-- 1-- ~ (5 , ~ > /

c: !

.2 40 ! / 10- ~ ; 1-- 1-- ..... t-- ~

fi) r !

c: " , Q)

~ c. 20 ,

fi) ~ ~ 1-- 1-- 1-- 1-- 1-- ~ ::l ; en h

/ !

"

0 ...L --'- ...L. ...L ... 4--. 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

1_4°C fœ10°C D20°C 1

Fig. J-7 Stability of Microcem 900 cement after 120 min .

• 100 900

-~ 80 0 -CI)

E ::l 60 0 > c: 0 40 en c: Cl) c. 20 UJ ::l en

0 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

j_4°C m10°C D20°C 1

• Fig. J-8 Final stability of Microcem 900 cement

1-5

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-~ 0 -Q)

E :l ë5 > c 0 'in c:: Q) Q. (/) ::J rn

100

80

60

40

20

o

Lanko 137

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

1_4°C ~20°C 1

Fig. J-9 Stability of Lanka 737 cement after 120 min .

-?f!. -Q)

E ::J 0 > c:: 0 cn c:: Q) Q. ", ::J rn

100

80

60

40

20

o

Lanko 137

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

1_4°C fl)20°C 1

Fig. J-10 Final stability of Lanko 737 cement

J~

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• 100 MC500+SP

r- ~r-- r' ~r--" ~ r

/ r" -'#. 80 1- ~ 1-- - ~ --- ~ ~ i--Q)

E ,., ::::::s 60 - ~ 1-- 1-- ~ - ~ ---0 /,

> c ~

, 1< f-0 40 - /, 1- k 1-- - - ~ ~ --"in -0

~ C , r

Q) r-

a. ~ " ,

fi) 20 - 1- .~ 1-- 'l - 'l. - ~ ~ ~ -::::::s r , "

cr" %

0 ~ ~ ... 4- ...1. ...1. ..l. + 4-, , 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

1_4°C Fi!J10°C D20°C 1

Fig. J-11 Stability of MC500 + SP cement after 120 min .

• MCSOO+SP 100

-~ 80 0 -Q)

E ::::::s 60 0 > c 0 40 'ëj; c Q) a. 20 fi) ::::::s

en 0

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

1_4°C fB10°C D20°C 1

• Fig. J-12 Stability of MC500 + SP cement

J·7

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100

-'if!. 80 -Q)

E ::s 60 o > c: .~ 40 c: Q)

~ 20 ::s en

A12

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. J-13 Stability of Spinor A 12 cement after 120 min .

100

-~ 80 -Q)

E ::s 60 g c: .~ 40 c: Q)

~ 20 ::s en

o

A12

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig J-14 Final stability of Spinor A 1 2 cement

Jo 8

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• 100 A16

'"' I-t- I-t-

-~ 80 l- i-- ~ 0 - ~ ~ 1-- ~ i-- 1"-

Q)

E ~ 60 ~ 1-- 1-- 1-- 1-- 1-- ~ 1--0 > c:: i

J. ~ 0 40 ~ f 1-- 1-- 1--

, ...... 1-- ~ ~ 1"-'u; /, 'i, /,

c:: : Q) a. 20 " fi) ~ ~

'/ 1-- ~ 1-- ~ ~

~ CI)

1,

0 ,

_1 i -~ 1 1 ~ ~ 1

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

1_4°C E 10°C D20°C 1

Fig. J-15 Stability of Spinor A 16 cement after 120 min.

• A16 100

-~ 80 -Q)

E ~ 60 '0 > c: 0 40 cn c:: Q) Q. 20 fi) ~

CI)

0 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

1_4°C œJ 10°C D20°C 1

• Fig. J-16 Final stability of Spinor A 16 cement

J-9

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100

-?F. 80 -Q)

E ~ 60 > c: .~ 40 c: Q)

~ 20 ::::s en

E12

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. J-17 Stability of Spinor E12 cement after 120 min .

100

-'$. 80 -Q)

E ::::s 60 ~ c: .Q 40 U) c: Q)

~ 20 ::::s en

E12

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. J-18 Final stability of Spinor E12 cement

J-IO

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APPENDIX K

SETllNG liME RESUL T8

K-l

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• 30 Type 10

25

F 20 ::l 0

15 .r:. -CI)

.E 10 ~

5

0 0 0.5 1 1.5 2

Initial W/C ratio

Fig. K-1 Initial setting time for Type 10 cement

• 30 Type 10

25

- 20 ~ ::J 0 .r:. 15 -CI)

E 10 t= 5

0 0 0.5 1 1.5 2

Initial W/C ratio

• Fig. K-2 Final setting time for Type 10 cement

K-2

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• 30 Type 30

25

~ 20 :::1

l15 ClJ E 10 i-

5

0

0 0.5 1 1.5 2 Initial W/C ratio

Fig. K-3 Initial setting time for Type 30 cement

• 30 Type 30

25

~ 20 :::1 0 é 15 ClJ E 10 ;::

5

0

0 0.5 1 1.5 2 Initial W/C ratio

• Fig. K-4 Final setting time for Type 30 cement

K-3

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• 30 650SR

25

~ 20 :l 0 ::S 15 Q)

E 10 i=

5

0

0 0.5 1 1.5 2 initial W/C ratio

Fig. K-5 Initial setting time for Microcem 650SR cement

• 30 650SR

25

~ 20 :l 0 5. 15 (1)

E 10 i=

5

0 0 0.5 1 1.5 2

Initial W/C ratio

• Fig. K-6 Final setting time for Microcem 650SR cement

K-4

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• 30 900

25

- 20 fi) - -:::s 0 .c 15 -Q)

E 10 ..... 5 h ~ ~ , o

o 0.5 1 1.5 2 Initial W/C ratio

Fig. K-7 Initial setting time for Microcem 900 cement

• 900 30

25

- 20 fi) -:::s 0 .r:. 15 -Q)

E 10 .... 5

0

0 0.5 1 1.5 " L

Initial W/C ratio

• Fig. K-8 Final setting time for Microcem 900 cement

K-5

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• Lanko 737 30

25

û) 20 ~

::::J 0 .c: 15 -cv E 10 ~

5

0

0 0.5 1 1.5 2 Initial W/C ratio

1--4°C "1!r 20°C 1

Fig. K-9 Initial setting time for Lanka 737 cement

• Lanko 7~.' 30

25

- 20 fi) ~

::::J 0 .r:. 15 -cv E 10 ~ <-~I

5

0

0 0.5 1 1.5 2 Initial W/C ratio

1--4°C "1!r 20°C 1

• Fig. K-10 Final setting time for Lanka 737 cement

K-6

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MC500" SP 30

25

Ci) 20 ~

~ 0 ~ 15 -Q)

.§ 10 .-5

0

a 0.5 1 1.5 2 Initial W/C ratio

1--4°C "* 1 aoc -A- 20°C 1

Fig. K-11 Initial setting time for MC500+ SP cement

MC500+SP 30 T--------------------------------, 25 +---------------------------------;

~ 20 +-----/~-/-4-"'-----------f

5. 15 +----~-_I_----------___i

~ 10 +-----,~~~;I~.-------------I 5 +---------------------__1 o ~~~~-+~~~~~---+-~~-+~~~~

o 0.5 1 1.5 2 Initial W/C ratio

Fig. K-12 Final setting time for MC500+ SP cement

K-7

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• A12 30

25

- 20 f!! ::::J 0

.s=. 15 -CI)

E 10 i=

5

0

0 0.5 1 1.5 2 Initial W/C ratio

1_4°C "* 10°C -6- 20°C 1

Fig. K-13 Initial setting time for Spinor A 12 cement

• A12 30

25

-f!! 20 ::::J

0 .s=. -CI) 15 E i=

10

5

0 0.5 1 1.5 2 Initial W/C ratio

1_4°C o 10°C -6- 20°C 1

• Fig. K-14 Final setting time for Spinor A12 cement

K-8

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30

25

(i) 20 ~

~ o .s 15 Q)

~ 10

5

o o

/ ,/

/' /

~

0.5

1

1 Initial W/C ratio

1_4°C *20°C 1

A12+SP(1,2',4)

. ,

1.5

Fig. K-15 Initial setting time for Spinor A 12 + SP cement

-

30

25

~ 20 ~ o .s 15 Q)

E 10 i-

5

o o

7 "" /'

7 /'

""

0.5 1 Initial W/C ratio

1_4°C *20°C 1

A 12+SP( 1,2',4)

1.5

Fig. K-16 Final setting time for Spinor A 12 + SP cement

K-9

2

2

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A16

30 ----------------------------------~

25+---------------~--------------~

~20+-----------~~--------------------1 ::::J o C 15 +_-----------7I(........--~I:io..-----------~~___1 Q) ç 10+-------~--~--~~------------~

5+-------~~=---------------------~

o o 0.5 1 1.5 2

Initial W1C ratio

Fig. K-17 Initial setting time for Spinor A 16 cement

A16 30?-------------------------------~

25 +-----------~=-------------------~

~20+------------+-----#-------~~--------t ::::J o C 15 +----------::If'-----+--~~-----------__1 Q)

.E 1 0 +---------.-.~+-----------------_I f-

5+-------~~----------------------__t

O+-~~~-+~~~~~~~~~~-+~~

o 0.5 1 1.5 2 Initial W/C ratio

Fig. K-18 Final setting time for Spinor A16+SP cement

K-lO

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• 30 E12

25

- 20 l!? ~ 0 .c: 15 ........ Q)

.§ 10 Jo-

5

0 0 0.5 1 1.5 2

Initial W/C ratio

Fig. K-19 Initial setting time for Spinor E12 cement

• 30 E12

25

~ 20 ~ 0 :S 15 Q)

E 10 i= 5

0

0 0.5 1 1.5 2 Initial W/C ratio

1. Fig. K-20 Final setting time for Spinor E12 cement

K-II

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• APPENDIX L

MODULUS OF ELASTICITY RESUL TS

• L-I

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• 20 T)'p! 10

-co Q. C!) 15 -2!' 'u ~ CI)

10 co Qi ..... 0 CI) :s 5 :s oc 0 ~

0

~ r"" I.~

0 '""' ~

~ ~ r-- - l-

Ii r..

p; l'"r-"

~ 1'>,

~ ...

... ~ - - ~ i-

.B !~

If .- 1.04- ---- ----

.L 1 . 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

Fig. L-' Modulus of elasticity vs. initial W/C ratio for Type 10 cement

• Type 30 20 -as a.

~ 15 ~ 'u ~ CI)

10 CU Qi ..... 0 CI) ::l 5 ::l oc 0 ~

0 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

• Fig. L-2 Modulus of elasticity vs. initial W/C ratio for Type 30 cement

L-2

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650SR 20------------------------------------

o 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

initial W/C ratio

Fig. L-3 Modulus of elasticity vs. initial \NIC ratio for Microcem E50SR cement

900 20T---------------------------------~ -lU

a.. ~ 15 ~ ë3 ~ : 10

'0 fi)

:::J 5 :::J 'C o ~

o 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

1 nitial W/C ratio

Fig. L-4 Modulus of elasticity vs. initial W/C ratio for Microcem 900 cement

L-3

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20

-cu a. ~ 15 ~ '0 +=i fi)

10 cu Ci) -0 fi) :::l 5 ~

"C 0 ~

0 0.4

Lanko 737

0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

1_4°C D20°C 1

Fig. L-5 Modulus of elasticity vs. initial 'NIC ratio for lanko 737 cement

20

-cu a. Q. 15 ~ 'C3 ~ fi)

10 cu Qi -0 fi) ~ 5 ~

"'C 0 ~

0 0.4 0.5

E12

0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

'_4°C D20°C 1

Fig. L-6 Modulus of elasticity vs. initiéd W/C ratio for Spinor E12 cement

L-4

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APPENDIX M

COMPRESSIVE STRENGTH RESUL TS

M-I

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Type 10 80 ,..----------------

60

-(\'S a. ~ 40 -

20

o 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

Fig. M-' Compressive strength vs. initial W/C ratio for Type 10 cement

80 ~-------------------------------Type 30

60

-CV a. ~ 40 '-'"

la 20

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. M-2 Compressive strength vs. initial W le ratio for Type 30 cement

M-2

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650SR 80--------------------------------~

60

-cu a.. :! 40 -~

20

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. M-3 Compressive strength vs. initial W/C ratio for Microcem 650SR cement

900 80 ----------------------------------

60 +-~----------------------------~ -cu a.. ~ 40 -

20

o 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

'_4°C D20°C 1

Fig. M-4 Compressive strength vs. initial W/C ratio for Microcem 900 cement

M-3

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Lanko 737 80~--------------------------------

60

-cu a.. ~ 40 -~

20

o 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

I:'~~b~~~ ~--------------------------------------------~

Fig. M-5 Compressive strength vs. initial W/C ratio for Lanko 737 cement

E12 80

60~--------------------------------~

-cu a.. ~ 40+-------------------------------~ -

20 +---

0+--+ 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

'_4°C D20°C 1

Fig. M-6 Compressive strength vs. initial W/C ratio for Spinor E12 cement

M-4

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APPENDIX N

SHRINKAGE/EXPANSION RESUL TS

N-I

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• Type 10

- 0.1 "#. 0 -c 0 -0.1 "Ci) c co -0.2 a. x Q) -0.3 -Q) 0> -0.4 co ~ c -0.5 .C:: ~ CI) -0.6

0 5 10 15 20 25 30 Curing time (days)

.. 2O°Cs (molslure = 100%) "* 20°C (molslure <30%)

-9- 4°C (molslure=100%) ... 4°C (molslure<30%)

Fig. N-' Shrinkage/expansion vs. curing time for Type 10 cement

• Type 30

- 0.1 ;:$? 0 - 0 c 0

"Ci) -0.1 c CO -0.2 a. X ~ -0.3 Q) 0>

-0.4 CO ~ c -0.5 .C:: ~ en -0.6

0 5 10 15 20 25 30 Curing time (days)

.. 2Q"Cs (molslure = 100%) "* 2O"C (moisI ure <30%)

-9- 4°C (molsture=100%) ... 4"C (molslure<30%)

• Fig. N-2 Shrinkage/expansion vs. curing time for Type 30 cement

N-2

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_ 0.1 '#. - o c: .~ ~0.1 c: ~ ~0.2 >< .~ ~0.3 Q) Cl co ~O.4 ~ c:

'C: ~O.5 .r:::. CI') ~0.6

o

Type 10SF

1,,;"'" - v_

~ ~ ~ --- -.........

.~

• • • • • • •

5 10 15 20 25 30 Curing time (days)

_ 20'CI (mOlllure = 100%) "'* 20'C (molilure <30% )

4 .'C (molSture=100%) ~ "'C (molsture<30'4)

Fig. N-3 Shrinkage/expansion vs. curing time for Type 10SF cement

650SR

- 0.1 ~ 0 0 -c: 0 -0.1 en c: co -0.2 CL )(

-~ ~~

.=:::--. .! -0.3 Q) C)

-0.4 co ~ c: -0.5 'C:

.r:::. en -0.6 • • · . • •

o 5 10 15 20 25 30 Curing time (days)

.. 20'CI (motllure = 100%) * 2Q'C (molSlure <30'4 )

-9- .'C (mOilture=100%) .. "'C (molsture<3Q'4)

Fig. N-4 Shrinkage/expansion vs. curing time for Microcem 650SR cement

N-3

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900

- 0.1 ~ 0

0 -c 0 -0.1 'u; c (\'J -0.2 c. )(

~ -0.3 Q) C)

-0.4 J2 c -0.5 ï= .c. en -0.6

0 5 10 15 20 25 30 Curing time (days)

_ 2O'Cs (mOlsture = 100%) '* 2O'C (molsture c:30% )

-9- 4'C (moisture=100%) .. 4'C (molsture<30%)

Fig. N-5 Shrinkage/expansion vs. curing time for Microcem 900 cement

_ 0.1 ?J!. - 0 c o 'in -0.1 c: ca c.

~ C) ca ~ c: 'i: .c: en

-0.2

-0.3

-0.4

-0.5

-0.6

A12

'" ,- ,-, v -- - - - ••

~ ~~

"- --- -e....

"'-

. • • . . o 5 10 15 20 25 30

Curing time (days) ... 2O'Cs (molsture = 100'11.) '* 2O'C (molslure <30% )

....... 4'C (molsture=100%) .. 4'C (molslure<30%)

Fig. N-6 Shrinkage/expansion vs. curing time for Spinor A 12 cement

N-4

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• MCSOO+SP

- 0.1 ':Ii!. 0 0 -c: 0 -0.1 'in c: co -0.2 0. )(

~ -0.3 C)

-0.4 co ~ c: -0.5 .~

.c en -0.6 0 5 10 15 20 25 30

Curing time (days) .. 2Q°Cs (molsture = 100%) * 2Q"C (molsture <30% )

-9- 4°C (molsture=1()(I'!l.) .. 4°C (molsture<3O%)

Fig, N-7 Shrinkage/expansion vs. curing time for MC500 + SP cement

• E12

- 0.1 'èJ?

0 -c: 0 -0.1 '0 c: cu -0.2 Q. )(

~ -0.3 C> -0.4 cu ~ c: -0.5 .~

.c. en -0.6

0 5 10 15 20 30 Curing time (da ys)

... 2O°Cs (molsture = 100%) * 20°C (molsture <30% )

...... 4"C (molsture=I00'!l.) .. 4°C (mOisture<30%)

• Fig. N-8 Shrinkage/expansion vs. curing time for Spinor E12 cement

N-5

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• APPENDIX 0

UL TRASONIC PULSE VELOCITY RESUL TS

• 0-1

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-fi)

E -.-~ '0 0 Q) > Q) > ~ ~

CU Q) .c CI)

Type 10 4000----------------------------~~

3000~------------------~

2000~~--=-----------------------~

1000

o 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

Fig. 0-1 Shear wave speed vs. initial W/C ratio at different temperatures for Type 10 cement

_ Type 10 CI) 4000 .....----------------......, E -~ '0 3000 o Q) > ~ ~ ~

"in fi)

! Q. E o u

2000

1000

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig.0-2 Compressive wave speed vs. initial W/C ratio at different temperatures for Type 10 cement

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4000 ~ ____________________________ ~_p_e_3_0_

-~ ~ 3000 ~-----------------t ëj o ~ ~ ~

2000 +-.rrt--

i 1000 Q) .c: (()

o 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

Fig. 0-3 Shear wave speed vs. initial W/C ratio at different tempe ratures for Type 30 cement

~ 4000 -~ '0 3000 o ~ Q)

> 2000 .... r~-~ ~

'c;; 1000 ri)

! a.

Type 30

5 0 u 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

1 nitial W/C ratio

Fig. 0-4 Compressive wave speed vs. initial W/C ratio at different temperatures for Type 30 cement

0-3

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650SR 4000------------------------------~ -~

:; 3000 +------------------1 '0 o G) > CI) > ~

2000

tu 1000 -"----""'"----Q) .r:. en

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

~!g 0-5 Shear wave speed vs. of initial W IC ratio at different temperatures for Microcem 650SR cement

I 4000

-~ '(j 3000 o G) > CI)

> 2000 ~ CI) > 'ii) 1000 U)

~ a. E

650SR

o 0 u 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

Fig. 0-6 Compressive wave speed vs. initial W/C ratio at different temperatures for Microcem 650SR cement

0-4

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4000 __ ------------------------------9°-°_ -~ -~ 3000r-----------------------------~

'0 0 Qj > Q) > ~ .... tU Q) ~ en

2000

1000

7-

'1 o +---L~-..a.Z ~""L.I-+-0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

Fig. 0-7 Shear wave speed vs. initial W le ratio at different temperatures for Microcem 900 cement

~ 4000 900

-~ '0 3000 o ~ CD > 2000 ~ ~ 'u; 1000 (1)

~ Co

~ 0 i----LJ-I-ILLJ~a;&..J_+_oo U 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

Fig. 0-8 Compressive wave speed vs. initial W IC ratio at different tempe ratures for Microcem 900 cement

0-5

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2500 -fi)

E 2000 -~ 'u

1500 0 Qj > CI)

1000 > ~ '-cu 500 CI)

.r::. en 0

Lanko 737

-r-

i--- - ~ -

- ~ -..L --+- .... +~ ,

0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig, 0-9 Shear wave speed vs. initial W/C ratio at different temperatures for Lanko 737 cement

-~ 4000 -~ '0 3000 o Q) > ~ ~ Q) >

2000

'iii 1000 tn ~ Q.

~ 0

Lanko 737

u 0.4 0.5 0.6 0.8 1.0 1.2 1.5 2.0 Initial W/C ratio

Fig. 0-10 Compressive wave speed vs. initial W/C ratio at different temperatures for Lanko 737 cement

0-6

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4000 E12

-fi) E - 3000 ~ '0 0 Qi

2000 > CI) > ~

1000 ~

(\1

r- -- r--- - -

CI) .t=. CI)

0 • -+ ~ + -+ ....L 1 . . • . 0.4 0.5 0.8 0.8 1.0 1.2 1.5 2.0

Initial W/C ratio

Fig. 0-11 Shear wave speed vs. initial W/C ratio at different temperatures for Spinor E 12 cement

- 4000 ~

E12

- r

~ '0 3000 0

t-

CI) > r-CI) > 2000 ~

~ - ~ r-

CI) > f;; 1000 fi) ~ - t---

~ Q. E 0 0 (J 4- ..1. .... 4- . .

• , , 0.4 0.5 0.8 0.8 1.0 1.2 1.5 2.0

1 nitial W/C ratio

Fig. 0-12Compressive wave speed vs. initial W/C ratio at different temperatures for Spinor E12 cement

0-7

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• APPENDIX P

MIXING TIME EFFECTS: RHEOLOGICAL PROPERTIES

• P-l

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Type 10 500 .... - 1 min fi)

Q. 400 -9-0 - 4 min .CI) -M-:t:: 300 fi) 10 mm 0 ..... 0 fi) 15 mm 'S; 200 CI) > +=i CU 100 Q) ct:

0 0 0.5 1 1.5

initial W/C ratio

Fig P-1 Relative viscosity of Type 10 cement at 0 min.

500

-fi) 400 Q. 0 -~ 300 fi) 0 0 fi)

'S; 200 CI) >

:t,'j cu

100 CI) ct:

0

Type 10

-1 min

+-------------------------------~~ 4mln

'*' +-------::::-"I~------------------~ 10 min .. 15 min

0 0.5 1 1.5 Initial W/C ratio

Fig. P-2 Relative viscosity of Type 10 cement at 60 min.

P-2

2

2

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• 500 Type 30 .. - 1 mm

t1J 400 ~ c.. 0 4 mm -~ *" 'ii) 300 10 mm 0 ... 0 15 min t1J '> 200 (J) > ~ m ëi) 100 tx:

0 0 0.5 1 1.5 2

1 nitial W/C ratio

Fig. P-3 Relative viscosity of Type 30 cement at 0 min.

• Type 30 500 .. - 1 mm f/J

0. 400 ...... & 4mln ~ '* cn 300 1Dmln 8 ... f/J 15 mm '5 200 (J) > ~ m

100 ëi) 0::

0

0 0.5 1 1.5 2 Initial W/C ratio

Fig. P-4 Relative viscosity of Type 30 cement at 60 min . • P-3

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500 Type10SF

-- 1 mm II)

400 Q. 09-(J - 4 min

~ '* '(ij 300 10mm 0 (J ... II)

15 min 'S; 200 Cl) >

+=' (\'S

100 Q) 0::

0 0 0.5 1 1.5

Initial W/C ratio

Fig. P-5 Relative viscosity of Type 10SF cement at 0 min,

500

..-fi)

400 c. 0 -..-~ 'CI) 300 0 (J fi)

'S; 200 Q) >

+=ï «1

100 ëii 0::

0

Type 10SF .. 1 mm

+-----~~--------------------._i~

4mm -M­

+-------~r__----------__f 10 mm

0 0.5 1 Initial W/C ratio

1.5

...... 15 min

Fig. P-6 Relative viscosity of Type 1 OSF cement at 60 min,

P-4

2

2

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-~ o -Cl)

E ~

o > c: o f/) c: Cl) a. f/) ~ en

100 Type 10

80

60

40

20

o 0.4 1.0 2.0

Initial W/C ratio

/_1 min lZJ4 min ~10 min 015 min

Fig. P-7 Suspension volume of Type 10 cement for different mixing time after 120 min

-~ o --Q)

E ::J o > c .0 U) c Q) ~ U) ::J

Cf)

100 Type 30

80

60

40

20

o 0.4 1.0 2.0

Initial W/C ratio

[.1 min 04 min ~10 min 015 min

Fig. P-8 Suspension volume of Type 30 cement for different mixing time aftvr 120 min

P-5

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100

-~ 80 Q)

E ~ 60 > c: .~ 40 c: Q)

~ 20 ::::s

(J)

o

Type10SF

0.4 1.0 2.0 Initial W/C ratio

1_1 min l[J4 min 010 min 015 min

Fig. P-9 Suspension volume of Type 10SF cement for different mixing time after 1 20 min

30 Type 10

-25 1 min r-...... 4 min - 20 ~

::::s * 1-10 min

0 s::;. 15 - ..

15 min 1-Q)

E 10 i=

5 ~ o .

o 0.5 1 1.5 2 Initial W/C ratio

Fig. P-10 Initial setting time for Tvpe 10 cement for different mixing times

P-6

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30

25

- 20 ~ ::J 0

..c. 15 -Q)

E 10 i=

5

0

Type 10 .. ....... -------------------t 1 min

-9-4 min

....... ----------------~~ 10 min ..

~--------_2JIA~:.._----___4 15 min

0 0.5 1 1.5 Initial W/C ratio

2

Fig. P-11 Final setting time for Type 10 cement for different mixing times

30 Type 30 ...

25 1 min 1-

-9-4 min - 20 tn '* 1-

'-::J 10 min 0 ..c. 15 -- ..

15 min Q)

E 10 i=

5 ~-d

.-1 • • . . o

o 0.5 1 1.5 2 1 nitial W/C ratio

Fig. P-12 Initial setting time for Type 30 cement for dîfferent mixing tîmes

P-7

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30 Type 30

~

25 -t----------------4 1 min .. - 20 ~ 4 min

-t-----------------------4~ :l 0 .r:: 15 -Q)

10 min

-t--------------------------4~ 15mln

E .- 10 t-

5

0

0 0.5 1 1.5 2 Initial W/C ratio

Fig. P-13 Final setting time for Type 30 cement for different mixing times

30 Type10SF ..

25 1 min f-.q.. 4 min - 20 t!!

:::s "* f-10 min

0 .r:: 15 - ....

15mln Q)

E .- 10 t-A

~~.--..

5 ......... -0 • .

o 0.5 1 1.5 2 Initial W/C ratio

Fig. P-14 Initial setting time for Type 10SF cement for different mixing times

P-8

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30 Type 10SF ..

25 +-_______________ --11 min

-9-4 min - 20 ~

~ +----------------------~~

10 min 0 .r:. 15 - ... +---------..,......-----------1 15 min Q)

E 10 j::

5

0 0 0.5 1 1.5 2

Initial W/C ratio

Fig. P-15 Final setting time for Type 10SF cement for different mixing times

P-9

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• APPENDIX Q

MIXING SPEEDS EFFECTS: RHEOLOGICAL PROPERTIES

• Q-l

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• 500 Type 10 ... - 750 RPM

(1) 400 .... Q. U 1500RPM -.a- * "in 300 2300RPM

8 ... CI) 3000RPM

:> 200 ~

Q) 6000RPM > :.e:= tU

ëD 100 a:::

0 0 0.5 1 1.5 2

Initial W/C ratio

Fig Q-' Relative viscosity of Type 10 cement at 0 min

• Type 10 500 .... - 750RPM m 400 Co ......

0 1500RPM -b "* cn 300 2300RPM

8 ... U) 3000RPM .:;

200 ... Q)

6000RPM > :.;::0 co ëii 100 0:::

a 0 0.5 1 1.5 2

Initial W/C ratio

Fig. Q-2 Relative viscosity of Type 10 cement at 60 min • Q-2

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• 500 Type 30

- ... fi)

400 750 Q. ~ .-~

1500

'üi 300 "*' 8 2300 fi) .... 'S; 200 3000

~ -&

+:0 600e CG

100 Qi Q:

0 0 0.5 1 1.5 2

Initial W/C ratio

Fig. Q-3 Relative viscosity of Type 30 cement at 0 min

• 500 Type 30

- ... fIJ 750 C. 400 0 -9-- 1500 ~ *' 'üi 300 8 2300

...... fIJ

3000 'S; 200 (1) -e->

+:0 6000

as 100 CI) 0::

0 0 0.5 1 1.5 2

Initial W/C ratio

• Fig. Q-4 Relative viscosity of Type 30 cement at 60 min

Q-3

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• 500 Type 10SF ... - 750 0 400 ...... c.

U 1500 -~ * 'ii) 300 2300 0 ... u 0 3000 :> 200 .. Q) 6000 > ~ lU

100 Qi a::

0 0 0.5 1 1.5 2

Initial W/C ratio

Fig. Q-5 Relative viscosity of Type 1 OSF ce~ent at 0 min

• Type10SF 500 ... - 750 0

C. 400 ...... u - 1500 ~ * cn 300 2300 8 .... 0 3000 '> 200 .. Q)

6000 > ~ cu

100 Qi a::

0 0 0.5 1 1.5 2

Initial W/C ratio

• Fig. Q-6 Relative viscosity of Type 10SF cement at 60 min

Q-4

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100 -?f!. 80 -Q)

E ::l 60 ë > c: 0 40 'ii) c: Q)

20 0-U) ::l

CI)

0

Typ.10

0.4 1.0 2.0 Initial W/C ratio

.750 RPM Ja1500 RPM [J2300 RPM 03000 RPM ~6000 RPM

Fig. Q-7 Suspension volume of Type 10 cement for different mixing speeds

100 -?f!. 80 -Q)

E ::l 60 ë > c: 0 40 'ii) c: Q) 0- 20 CI) ::l

CI)

0

Type 30

0.4 1.0 2.0 1 nitial W/C ratio

.750 RPM 181500 RPM ~2300 RPM 03000 RPM ~6000 RPM

Fig. Q-8 Suspension volume of Typa 30 cement for different mixing speeds

Q-S

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-~ 0 -CI)

E j

ë5 > c 0 fi; c CI) Co ", j

CI)

100

80

60

40

20

0

Type 10SF

0.4 1.0 2.0 Initial W/C ratio

.750RPM FB1500RPM ~2300RPM 03000 RPM ~6000 RPM

Fig. Q-9 Suspension volume of Type 10SF cement for different mixing speeds

30 Type 10

-25 750RPM 09-- 20 f!! 1500 RPM -Mo

::l 0 .c 15 -Q)

E 10 ~

2300 RPM .... 3000 RPM 0&-

~ 6000RPM

5

0 ~ . . . . o 0.5 1 1.5 2

Initial W/C ratio

Fig. Q-10lnitial setting time for Type 10 cement for different mixing speeds

Q~

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20 Type 10

... 750 ~PM

15 -9-- 1500 RPM

~ +1-::J 2300 RPM 0 -.. ~ 10 - 3000 RPM Q) e-E i= 6000 RPM

5

o 0.5 1 1.5 2 Initial W/C ratio

Fig. Q-11 Final setting time for Type 10 cement for different mixing speeds

30

25

'? 20 :::J o S. 15 Q)

E .- 10 1--

5

o ....--

o 0.5

Type 30 .. 750 RPM 009-1500 RPM

"* 2300 RPM ...-3000 RPM -& 6000 RPM

~ ~

• . 1 1.5 2

Initial W/C ratio

Fig. Q-12lnitial setting time for Type 30 cement for different mixing speeds

Q-7

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30

25

- 20 ~ ~ 0 .r:. 15 "-Q)

E .- 10 ~

5

0

Type 30

.-+-_____________ """"1750 RPM

09-1500RPM

+---------------------~~ 2300RPM

"* +---------~-----~ 3000RPM

-e­~--------,,~~-------_t 6000 RPM

0 0.5 1 1.5 Initial W/C ratio

2

Fig. Q-13 Final setting tÎme for Type 30 cement for different mixing speeds

30 Type 10SF

.-25 750 RPM

-9-- 20 ~ 1500 RPM

* ~ 0

.r:. 15 -CI)

E 10 t=

5

2300 RPM ... 3000 RPM -e-

JiW' 6000RPM

~ o --'-

o 0.5 1 1.5 2 Initial W/C ratio

Fig. Q-14lnitial setting time for Type 10SF cement for different mixing speeds

Q.g

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Type 10SF 30T---------------------------------~ .. 25 ~----------------------------~750RPM

09-1500 RPM

~20~------------------------~* ::::J 2300 RPM o ~15 • 3000 RPM ~ ~ E .- 1 0 6000 RPM 1-

5 +-------------------------------------~

o +-~~~+4~~~_+~~_+~+_~~+_~~ o 0.5 1 1.5 2

Initial W/C ratio

Fig. Q-15Final setting time for Type 10SF cement for different mixing speeds

Q-9


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