Rheological Properties of Lihir Ore
Rheological Properties of Lihir Ore
Rheological Properties of Lihir Ore
ii
exception of one Newtonian sample) indicated time independ ent shear
thinning with yield stress. Time independency, thixotropy and anti -
thixotropy were observed; the precise behaviour was dependent on
both the sample and sample concentration.
iii
Declaration by author
This thesis is composed of my original work, and contains no
material previously published or written by anot her person except
where due reference has been made in the text. I have clearly stated
the contribution by others to jointly -authored works that I have
included in my thesis.
iv
holder to reproduce material i n this thesis and have sought permission
from co-authors for any jointly authored works included in the thesis.
v
Publications included in this thesis
No publications included.
vi
My supervisors, Frank Shi and Yongjun Peng, conceived this
project and helped with experimental design and the interpretation of
experimental data.
vii
Acknowledgements
Numerous people have helped me in one way or another through
this project:
o Maruf
o John
viii
o Daniel
o Raoni
o Ditend
ix
• Ding for assisting me with the sedimentation analysis
x
Financial support
This project was generously supported by Newcrest Mining
Limited.
Keywords
Rheology, sedimentation, viscosity, mining, gold ore, & clay
xi
Dedication
I dedicate with love this thesis to my wife Kirsti. Your love and
kindness supported me throughout this very challenging chapter in my
life; you were vital to me staying the course and completing this
degree. Now it’s your turn!
xii
Contents
Abstract .............................................................................................................................................................. ii
Declaration by author ........................................................................................................................................ iv
Publications included in this thesis ................................................................................................................... vi
Submitted manuscripts included in this thesis.................................................................................................. vi
Other publications during candidature ............................................................................................................. vi
Contributions by others to the thesis ................................................................................................................ vi
Statement of parts of the thesis submitted to qualify for the award of another degree ................................ vii
Research Involving Human or Animal Subjects ................................................................................................ vii
Acknowledgements ......................................................................................................................................... viii
Financial support ............................................................................................................................................... xi
Keywords ........................................................................................................................................................... xi
Australian and New Zealand Standard Research Classifications (ANZSRC)....................................................... xi
Fields of Research (FoR) Classification .............................................................................................................. xi
Dedication......................................................................................................................................................... xii
Contents .......................................................................................................................................................... xiii
Table of figures .............................................................................................................................................. xviii
Table of tables ............................................................................................................................................... xxiii
List of abbreviations ....................................................................................................................................... xxv
Chapter 1 Introduction ................................................................................................................................... 1
1.1 Background ........................................................................................................................................ 1
1.2 Aims and objectives ........................................................................................................................... 2
1.3 Statement of Sustainability ............................................................................................................... 3
1.4 Thesis structure overview.................................................................................................................. 3
Chapter 2 Literature Review .......................................................................................................................... 5
2.1 Lihir ore .............................................................................................................................................. 5
2.2 Background on rheology theory ........................................................................................................ 8
2.2.1 Time independent behaviour .................................................................................................... 9
2.2.2 Time dependent behaviour ..................................................................................................... 10
2.3 Effect of solids concentration on viscosity ...................................................................................... 13
2.4 Rheology dependency ..................................................................................................................... 16
2.4.1 Solids concentration ................................................................................................................ 17
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2.4.2 Particle size distribution .......................................................................................................... 20
2.4.3 Chemical environment ............................................................................................................ 21
2.4.4 Temperature ............................................................................................................................ 24
2.5 Flow models and the importance of using them............................................................................. 25
2.6 Rheometer selection ....................................................................................................................... 26
2.6.1 Parallel Plate ............................................................................................................................ 26
2.6.2 Cone and plate......................................................................................................................... 27
2.6.3 Coaxial cylinder or ‘cup and bob’ ............................................................................................ 28
2.6.4 Vane ......................................................................................................................................... 29
2.6.5 Capillary rheometer ................................................................................................................. 31
2.6.6 Summary .................................................................................................................................. 32
2.7 Coaxial cylinder shear rate calculations .......................................................................................... 33
2.7.1 Narrow gap .............................................................................................................................. 33
2.7.2 Infinite sea ............................................................................................................................... 35
2.7.3 Krieger approximate solution .................................................................................................. 36
2.7.4 Estelle et al Bingham approximation ....................................................................................... 36
2.8 Measuring the rheology of settling slurries..................................................................................... 37
2.8.1 Elongated coaxial cylinders ..................................................................................................... 39
2.8.2 Debex ....................................................................................................................................... 40
2.8.3 Akroyd-Nguyen helical flow rheometer .................................................................................. 42
2.9 Clay mineralogy ............................................................................................................................... 44
2.9.1 Clay .......................................................................................................................................... 45
2.9.2 Lihir Clays ................................................................................................................................. 49
2.9.3 Rheology measurements of slurries with high clay contents .................................................. 53
2.9.4 Time dependency in clay suspensions..................................................................................... 54
2.9.5 Accurate sizing of clay particles ............................................................................................... 58
2.10 Rheology’s effect on mineral processing performance ................................................................... 59
2.10.1 Grinding circuit ........................................................................................................................ 59
2.10.2 Flotation................................................................................................................................... 62
2.10.3 Other mineral processes.......................................................................................................... 64
2.11 Sedimentation of mineral ores ........................................................................................................ 64
2.12 Predicting Lihir ore slurry rheology ................................................................................................. 66
2.13 Gaps in the literature....................................................................................................................... 68
Chapter 3 Testing rig and rheometer commissioning .................................................................................. 70
xiv
3.1 Design considerations common to both helical flow rheometry and coaxial flow rheometry ....... 71
3.1.1 Sample stability ....................................................................................................................... 72
3.1.2 Predicting if a flow curve is producible with a given rheometer............................................. 73
3.2 Helical flow rheometer commissioning ........................................................................................... 75
3.2.1 Measuring chamber................................................................................................................. 77
3.2.2 Pump........................................................................................................................................ 79
3.2.3 Sump ........................................................................................................................................ 80
3.2.4 Testing rig operation ............................................................................................................... 81
3.3 Rheometer selection ....................................................................................................................... 82
3.3.1 Selection of the HAAKE Viscometer ........................................................................................ 82
3.3.2 Alternative rheometers ........................................................................................................... 82
3.3.3 Anton Paar ............................................................................................................................... 83
3.4 RM180 co-axial cup commissioning ................................................................................................ 84
3.4.1 Time dependency .................................................................................................................... 85
3.5 Summary of design considerations ................................................................................................. 87
Chapter 4 Experimental methodology ......................................................................................................... 89
4.1 Data entry ........................................................................................................................................ 89
4.2 Materials .......................................................................................................................................... 89
4.3 Particle sizing ................................................................................................................................... 90
4.4 Sample preparation ......................................................................................................................... 91
4.4.1 Splitting .................................................................................................................................... 92
4.4.2 Grinding procedure ................................................................................................................. 93
4.5 Sedimentation tests......................................................................................................................... 94
4.6 Measuring pH, dissolved oxygen, and temperature ....................................................................... 95
4.7 HAAKE experimental procedure ...................................................................................................... 95
4.7.1 Premixing the slurry and loading the helical flow rheometer ................................................. 96
4.7.2 Rheology test ........................................................................................................................... 97
4.7.3 Flow rate .................................................................................................................................. 97
4.7.4 Adjusting sample concentration .............................................................................................. 97
4.8 RM180 experimental procedure ..................................................................................................... 98
4.8.1 Mixing the sample ................................................................................................................... 99
4.8.2 Loading and unloading the rheometer .................................................................................... 99
4.8.3 Selecting a bob ...................................................................................................................... 100
4.8.4 Yield stress tests .................................................................................................................... 102
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4.8.5 Rheology test: Ramping procedure ....................................................................................... 103
4.8.6 Benefits and limitations ......................................................................................................... 103
4.9 Data reduction ............................................................................................................................... 104
4.9.1 Coaxial cylinder ...................................................................................................................... 104
4.9.2 Modified Estelle method ....................................................................................................... 105
4.9.3 Turbulence ............................................................................................................................. 114
4.9.4 Casson approximation ........................................................................................................... 114
4.10 Summary........................................................................................................................................ 116
Chapter 5 Test results................................................................................................................................. 118
5.1 RM180 calibration and validation of the final testing procedure ................................................. 118
5.2 Confirmation that the master sizing is comparable to sieving ...................................................... 121
5.3 Particle size and size distribution .................................................................................................. 122
5.4 Summary of the rheology and sedimentation data ...................................................................... 128
5.5 Summary of test results................................................................................................................. 132
Chapter 6 Analysis of the slurry rheology .................................................................................................. 134
6.1 Time dependency .......................................................................................................................... 134
6.1.1 Advanced argillic .................................................................................................................... 139
6.1.2 Argillic .................................................................................................................................... 139
6.1.3 Upper epithermal .................................................................................................................. 139
6.1.4 Silica breccia .......................................................................................................................... 140
6.1.5 Lower epithermal .................................................................................................................. 141
6.1.6 Outer biotite .......................................................................................................................... 142
6.1.7 Inner biotite ........................................................................................................................... 142
6.1.8 Comparison to other materials ............................................................................................. 143
6.2 Solids concentration effect on yield stress and viscosity .............................................................. 144
6.3 Grinding effect ............................................................................................................................... 146
6.4 Domain .......................................................................................................................................... 153
6.5 The dependence on ore characteristics ........................................................................................ 160
6.6 Multilinear regression ................................................................................................................... 163
6.7 Summary........................................................................................................................................ 172
Chapter 7 Analysis of slurry stability .......................................................................................................... 174
7.1 Concentration effect...................................................................................................................... 174
7.2 Alteration domain.......................................................................................................................... 175
7.3 Particle size and particle size distribution ..................................................................................... 176
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7.4 Swelling.......................................................................................................................................... 178
7.5 Sedimentation rate and time delay ............................................................................................... 180
7.6 Apparent viscosity and sedimentation rate .................................................................................. 181
7.7 Slurry stability and time-dependency ........................................................................................... 184
Chapter 8 Conclusion and further work ..................................................................................................... 185
8.1 Summary of equipment design ..................................................................................................... 185
8.2 Summary of major research findings ............................................................................................ 186
8.3 Future work ................................................................................................................................... 189
References ..................................................................................................................................................... 192
Appendixes Overview .................................................................................................................................... 197
Appendix A Sequence list .......................................................................................................................... 198
Appendix B Tables of rheology and sedimentation data .......................................................................... 213
A.1: Advanced argillic............................................................................................................................ 213
A.2: Argillic ............................................................................................................................................ 214
A.3: Upper epithermal samples ............................................................................................................ 220
A.4: Silica Breccia .................................................................................................................................. 229
A.5: Lower Epithermal .......................................................................................................................... 234
A.6: Outer biotite .................................................................................................................................. 240
A.7: Inner biotite ................................................................................................................................... 252
Appendix C Statistical results .................................................................................................................... 258
A.8: Regression analysis of apparent viscosity vs pH, concentration, passing 9.86, passing 38, passing
53, amorphous silicate, kaolinite and clay content ................................................................................... 258
A.9: Regression analysis of the logarithm of apparent viscosity vs pH, concentration, passing 9.86,
passing 38, passing 53, amorphous silicate, kaolinite and clay content ................................................... 262
Appendix D Sizing data .............................................................................................................................. 267
Appendix E Data processing example including raw data ........................................................................ 275
A.10: Estelle method ........................................................................................................................... 281
A.11: Casson approximation ............................................................................................................... 294
A.12: Summary .................................................................................................................................... 302
A.13: Raw data for SEQ233 ................................................................................................................. 304
Appendix F Sedimentation curves ............................................................................................................ 323
Appendix G Flow curves ............................................................................................................................ 324
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Table of figures
Figure 2-1: Schematic approximation of variation in Lihir mineralogy as
taken from Gardner (2016). The new domains currently used by Newcrest
may be seen on the lower horizontal axis whilst the older domain
characterisation is on the upper horizontal axis. The y -axis is the weight
p e r c e n t a g e ( w t % ) ................................................................................................................................... 6
Figure 2-2: Pyrite value classification diagram. No chemical or textural
s p a t i a l d i s t i n c t i o n e s t a b l i s h e d . T a k e n f r o m ( G a r d n e r , 2 0 1 6 ) . ................................ 8
Figure 2-3: Flow curves for time-independent slurries. Taken from
( K l i m p e l , 1 9 8 4 ) . ..................................................................................................................................... 9
Figure 2-4: The loop and step tests for determining time -dependent
r h e o l o g i c a l b e h a v i o u r . T a k e n f r o m ( T a d r o s , 2 0 1 0 ) ...................................................... 13
Figure 2-5 : Mendoza (2017) plot of relative viscosity; the predicted
values are represented by the lines and the experimental values by the
s y m b o l s ....................................................................................................................................................... 15
F i g u r e 2 - 6 : T h i x o t r o p y o f i r o n m i n e t a i l i n g s l u r r y ( J e o n g e t a l . , 2 0 1 5 ) ....... 17
F i g u r e 2 - 7 : S h i ( 1 9 9 5 ) s i m u l a t e d f l o w c u r v e s o f H e l l y e r g r i n d i n g s l u r r y . .. 19
Figure 2-8: Flow curves of discharge slurries of Emu Gold ball mills. As
can be seen (a) is dilatant with low yiel d stress whilst (b) is Pseudoplastic
w i t h h i g h y i e l d s t r e s s . T a k e n f r o m S h i ( 2 0 0 2 ) . .............................................................. 21
Figure 2-9: Effect of low molecular weight polyacrylic acid on the shear
yield stress-pH behaviour for a zirconia suspension at 57% (wt%) (Boger,
2 0 0 9 ) ............................................................................................................................................................ 23
Figure 2-10: Zirconia suspension with additive of polyacrylic at 57% with
u n a d j u s t e d p H a n d 8 8 . 7 % w i t h a d j u s t e d p H ( B o g e r , 2 0 0 9 ) . ................................... 24
F i g u r e 2 - 1 1 : P a r a l l e l p l a t e ( A n o n , 2 0 1 6 ) ............................................................................ 26
F i g u r e 2 - 1 2 : C o n e a n d p l a t e ( A n o n , 2 0 1 6 ) ......................................................................... 27
Figure 2-13:DIN 53019 / ISO 3219 coaxial cylinder geometry (Anon, 2016)
......................................................................................................................................................................... 28
F i g u r e 2 - 1 4 : V a n e G e o m e t r i e s ( A n o n , 2 0 1 6 ) .................................................................... 30
F i g u r e 2 - 1 5 : C a p i l l a r y r h e o m e t e r s c h e m a t i c ( A k r o y d , 2 0 0 4 ) .................................. 32
F i g u r e 2 - 1 6 : C o a x i a l c y l i n d e r i m a g e t a k e n f r o m I S O ( 1 9 9 5 ) ................................ 35
Figure 2-17: A schematic showing particle settling zones formed in a
c o n v e n t i o n a l c u p a n d b o b r h e o m e t e r ( K l e i n e t a l . , 1 9 9 5 ) ........................................ 38
Figure 2-18: Rheological measurements of a fly ash slurry using a standard
b o b a n d c u p g e o m e t r y ( A k r o y d , 2 0 0 4 ) . ................................................................................. 39
Figure 2-19: The Klein et al (1995) solution to measuring the rheology of
s e t t l i n g s l u r r i e s . .................................................................................................................................. 40
Figure 2-20: A schematic of a testing rig built on the same principles as
t h e D e b e x r h e o m e t e r ( S h i , 2 0 1 6 ) .............................................................................................. 41
F i g u r e 2 - 2 1 : A p r e v i o u s v i s c o s i t y t e s t i n g r i g u s e d b y S h i ( 2 0 1 6 ) ..................... 41
Figure 2-22: A schematic used as the base of the design of the Akroyd
( 2 0 0 4 ) h e l i c a l f l o w r h e o m e t e r .................................................................................................... 43
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Figure 2-23 Error in shear rate between flow rheometer data analysed using
helical flow and Couette flow theory for a 1 wt% CMC solution (taken fr om
A k r o y d ( 2 0 0 4 ) ) ...................................................................................................................................... 44
Figure 2-24: Apparent viscosity of quartz and amorphous silica
suspensions at 100s-1 as a function of solids concentration (Chen et al.,
2 0 1 7 ) ............................................................................................................................................................ 45
Figure 2-25: Diagram showing a clay mineral layer (A); a particle (B); an
aggregate (c); and an assembly of aggregates (D) (taken from Bergaya and
L a g a l y ( 2 0 1 3 ) ) . ..................................................................................................................................... 47
Figure 2-26:edge/face and face/face contacts that link the particles to a
h o u s e o f c a r d s ( a ) o r a b a n d - l i k e ( b ) s t r u c t u r e ( L a g a l y , 1 9 8 9 ) . ......................... 48
Figure 2-27:A classification of phyllosilicate clay minerals (Ndlovu, 2014)
......................................................................................................................................................................... 49
Figure 2-28: Viscosity ternary plots in volumetric fractions at ph7. Note,
that the plots are a different solid concentration; the solids are at 15% and
30% volumetric concentration for the graphs on the left and right
r e s p e c t i v e l y . ........................................................................................................................................... 52
Figure 2-29: Time dependent viscosity of nuclear waste slurries showing
thixotropic, anti-thixotropic and time independent behaviour under
d i f f e r e n t s h e a r r a t e s ( S m i t h e t a l . , 2 0 0 0 ) . ......................................................................... 54
Figure 2-30: Viscosity against time for 1997 ppm partially hydrolysed
p o l y a c r y l a m i d e i n w a t e r / g l y c e r i n e ( B u i t e n h u i s a n d S p r i n g e r , 2 0 0 3 ) ............... 55
Figure 2-31: Flow curve for a thixotropic yield -stress fluid experiencing
bifurcation contrasted against an ideal yield stress fluid (Coussot et al.,
2 0 0 2 ) . .......................................................................................................................................................... 56
Figure 2-32: shear rate versus time for a 4.5% bentonite suspension after
20s of rest following an intense 60s of 26 Pa pre -shear using a vane in cup
g e o m e t r y . .................................................................................................................................................. 57
Figure 2-33: Comparison of different sizing techniques (Napier -Munn et
a l . , 1 9 9 6 ) ................................................................................................................................................... 59
F i g u r e 2 - 3 4 : T h e f l o t a t i o n p r o c e s s . T a k e n f r o m L i ( 2 0 1 6 ) ..................................... 63
Figure 2-35: Ferrosilicon sedimentation rate at a variety of densities (Shi,
2 0 1 6 ) ............................................................................................................................................................ 66
F i g u r e 3 - 1 : T h e f i r s t i t e r a t i o n o f t h e n e w t e s t i n g r i g ................................................ 76
F i g u r e 3 - 2 : T h e c u r r e n t t e s t i n g r i g ......................................................................................... 77
Figure 3-3: Cumulative percent passing stated size in various processes of
L i h i r ' s g r i n d i n g c i r c u i t ( S h i , 2 0 1 7 a ) ...................................................................................... 78
Figure 3-4:HAAKE rheometer running a calibration test. Immersion tube
w a s u s e d f o r a n a r r o w g a p g e o m e t r y . ..................................................................................... 79
Figure 4-1: Particle size distribution curves of NTS050 after grinding for a
d i f f e r e n t i a l a m o u n t o f t i m e . ......................................................................................................... 94
F i g u r e 4 - 2 : S m a l l b o b a n d l a r g e b o b u s e d i n R M 1 8 0 r h e o m e t e r . ........................ 101
F i g u r e 4 - 3 : A n g u l a r s p e e d v s t o r q u e f o r S E Q 2 3 3 . ...................................................... 107
Figure 4-4: Comparison between the Casson approximation and the Estelle
method using a 6th order polynomial fit of Ω(M). The data was from
S E Q 2 3 3 . ................................................................................................................................................... 112
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Figure 4-5: Fitting a Casson model to the Estelle approximation of SEQ233
u s i n g a 6 t h o r d e r p o l y n o m i a l f i t o f Ω ( M ) . ......................................................................... 113
Figure 5-1: Calibration of the RM180 using 486 mPa.s Newtonian oil (prior
t o c o r r e c t i o n f a c t o r s ) . .................................................................................................................... 119
Figure 5-2: NTS100 53% (v/v) Comparison of raw results for the larg e bob
....................................................................................................................................................................... 120
F i g u r e 5 - 3 : R e p e a t o f N T S 0 5 4 u s i n g f r e s h s a m p l e s ................................................... 121
Figure 5-4: Comparison of the Malvern MasterSizer to wet sieving bel ow
3 8 μ m . ....................................................................................................................................................... 122
F i g u r e 5 - 5 : O u t e r b i o t i t e c u m u l a t i v e p a s s i n g s i z e ....................................................... 123
F i g u r e 5 - 6 : N T S 1 1 0 a t 4 6 % ( v / v ) a f t e r 5 m i n u t e s o f g r i n d i n g . .......................... 132
F i g u r e 6 - 1 : N T S 0 5 4 a t 5 7 % s o l i d v o l u m e t r i c c o n c e n t r a t i o n . .............................. 135
F i g u r e 6 - 2 : N T S 1 0 8 a t 4 6 % s o l i d v o l u m e t r i c c o n c e n t r a t i o n . .............................. 135
Figure 6-3: Raw data of the hysteresis loop conducted on NTS108
( S e q u e n c e 2 3 1 w i t h a s o l i d v o l u m e t r i c c o n c e n t r a t i o n o f 4 6 % ) .......................... 136
Figure 6-4: The raw data of NTS108 (SEQ231) at a solid concentration of
4 6 % ( v / v ) b e i n g s h e a r e d b y t h e s m a l l b o b a t 9 9 9 r o t a t i o n s p e r m i n u t e . ...... 137
Figure 6-5:The change in the “yield stress” of an argillic sa mple (NTS109
at 53% concentration; SEQ400) prior to the first, second, and third loop
t e s t . ............................................................................................................................................................. 138
Figure 6-6: The increase in yield stress over time of NTS111 (after
g r i n d i n g a n d a t 4 6 % s o l i d v o l u m e t r i c c o n c e n t r a t i o n ) . ............................................. 140
Figure 6-7: Apparent viscosity (at a shear rate of 50 s -1) in relation to
s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r a r g i l l i c s a m p l e N T S 1 0 8 . ............................... 144
Figure 6-8: Flow curves of NTS008 (upper epithermal) at 53% and 46%
s o l i d s c o n c e n t r a t i o n ( v / v ) . .......................................................................................................... 145
Figure 6-9: The grinding effect on the relationship of slurry viscosity with
s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r o u t e r b i o t i t e ( N T S 0 5 4 ) .................................. 148
Figure 6-10: The grinding effect on the relationship of slurry viscosity
w i t h s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r i n n e r b i o t i t e ( N T S 0 9 7 ) ...................... 149
Figure 6-11: The grinding effect on the relationship of slurry viscosity
w i t h s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r a r g i l l i c ( N T S 1 0 8 ) .................................. 150
Figure 6-12: The grinding effect on the relationship of slurry viscosity
w i t h s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r l o w e r e p i t h e r m a l N T S 1 1 0 ................ 151
Figure 6-13: The grinding effect on the relationship of slurry viscosity
w i t h s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r u p p e r e p i t h e r m a l ( N T S 1 1 1 ) ............ 152
Figure 6-14: Apparent viscosity (at a shear rate of 50 s -1) in relation to
s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r a d v a n c e d a r g i l l i c s a m p l e N T S 0 3 7 . ........ 153
Figure 6-15: Apparent viscosity (at a shear rate of 50 s-1) in relation to
s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r a r g i l l i c s a m p l e s .................................................. 154
Figure 6-16: Apparent viscosity (at a shear rate of 50 s-1) in relation to
s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r u p p e r e p i t h e r m a l s a m p l e s ............................ 155
Figure 6-17: Apparent viscosity (at a shear rate of 50 s -1) in relation to
s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r s i l i c a b r e c c i a s a m p l e s .................................... 156
Figure 6-18: Apparent viscosity (at a shear rate of 50 s-1) in relation to
s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r u p p e r l o w e r e p i t h e r m a l ................................. 156
xx
Figure 6-19: Apparent viscosity (at a shear rate of 50 s -1) in relation to
s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r i n n e r b i o t i t e s a m p l e s . .................................... 157
Figure 6-20: Apparent viscosity (at a shear rate of 50 s -1) in relation to
s o l i d v o l u m e t r i c c o n c e n t r a t i o n f o r o u t e r b i o t i t e s a m p l e s ...................................... 158
Figure 6-21: Slurry viscosities of various samples at a constant 46% solid
v o l u m e t r i c c o n c e n t r a t i o n . ............................................................................................................ 159
F i g u r e 6 - 2 2 : S l u r r y v i s c o s i t y i n r e l a t i o n t o p H f o r a l l t e s t e d s a m p l e s ........ 162
Figure 6-23: Minitab graph of the multilinear regression results against the
f i t t e d v a l u e s .......................................................................................................................................... 164
Figure 6-24: Minitab results of the fitted multilinear results against the
m e a s u r e d a p p a r e n t v i s c o s i t y a t 5 0 s - 1 . ................................................................................ 164
Figure 6-25: The predicted vs measured natural logarithms of the apparent
v i s c o s i t y a t 5 0 s - 1 . .............................................................................................................................. 165
Figure 6-26: Minitab’s four in one chart showing the residuals relationship
w i t h t h e l o g a r i t h m o f t h e a p p a r e n t v i s c o s i t y . ................................................................ 166
Figure 6-27: Surface plot of the logarithm of apparent viscosity at 50s -1 vs
c o n c e n t r a t i o n a n d p H . .................................................................................................................... 168
Figure 6-28: Surface plot of the logarithm of vi scosity at 50 s-1 vs the
p a r t i c l e s i z e s s m a l l e r t h a n 9 . 8 6 µ m a n d t h e a m o r p h o u s s i l i c a c o n t e n t . ....... 169
Figure 6-29: Surface plot of the logarithm of viscosity at 50 s-1 vs the clay
c o n t e n t a n d t h e p H ............................................................................................................................ 169
Figure 6-30: Surface plot of the logarithm of viscosity at 50 s -1 vs the
p a r t i c l e s i z e s s m a l l e r t h a n 9 . 8 6 µ m a n d t h e p H ............................................................ 170
Figure 6-31: Surface plot of the logarithm of viscosity at 50 s-1 vs the
K a o l i n i t e c o n t e n t a n d t h e p H ..................................................................................................... 171
Figure 7-1: Average sedimentation rate in relation to solid volumetric
c o n c e n t r a t i o n f o r N T S 0 0 8 ............................................................................................................ 175
Figure 7-2:Comparison of highest concentrations when sedimentation above
2 m L / h o u r w a s o b s e r v e d ............................................................................................................ 176
Figure 7-3: Sedimentation rate in relation to solid volumetric
c o n c e n t r a t i o n f o r a r g i l l i c o r e s a m p l e s . .............................................................................. 177
Figure 7-4:An example of a swelling sample, during sedimentation
m e a s u r e m e n t o v e r 3 . 4 h o u r s ....................................................................................................... 178
Figure 7-5:The volume of the mud-line over time in the sedimentation
m e a s u r e m e n t f o r N T S 0 0 8 a t 5 5 % s o l i d v o l u m e t r i c c o n c e n t r a t i o n . ................... 180
Figure 7-6: Time delay in the sedimentation process for NTS008 sample
after one, twelve and twenty-four minutes after starting the sedimentation
e x p e r i m e n t . ............................................................................................................................................ 181
Figure 7-7: Slurry viscosity in relation to sedimentation rate for the entire
o r e s a m p l e s ............................................................................................................................................ 182
Figure 7-8: Linear regression on the data of slurry viscosity in relation to
s e d i m e n t a t i o n r a t e f o r t h e e n t i r e o r e s a m p l e s ................................................................ 183
F i g u r e D - 1 : A d v a n c e d a r g i l l i c c u m u l a t i v e p a s s i n g s i z e ........................................... 271
F i g u r e D - 2 : A r g i l l i c c u m u l a t i v e p a s s i n g s i z e ................................................................ 272
F i g u r e D - 3 : U p p e r e p i t h e r m a l c u m u l a t i v e p a s s i n g s i z e ............................................ 272
F i g u r e D - 4 : S i l i c a b r e c c i a c u m u l a t i v e p a s s i n g s i z e .................................................... 273
xxi
F i g u r e D - 5 : U p p e r e p i t h e r m a l c u m u l a t i v e p a s s i n g s i z e ........................................... 273
F i g u r e D - 6 : I n n e r b i o t i t e c u m u l a t i v e p a s s i n g s i z e ....................................................... 275
Figure E-1: A comparison of the predicted vs measured angula r velocity
w h e r e 𝛺𝑃 i s t h e p r e d i c t e d a n g u l a r v e l o c i t y a n d 𝛺𝐸 i s t h e e x p e r i m e n t a l
a n g u l a r v e l o c i t y . ................................................................................................................................ 301
Figure E-2: A comparison of the different rheograms produced by the
d i f f e r e n t m e t h o d s . ............................................................................................................................. 303
xxii
Table of tables
T a b l e 2 - 1 : T h e a v e r a g e g o l d a n d s u l p h u r c o n t e n t o f t h e L i h i r o r e ' t y p e s ' ..... 7
T a b l e 3 - 1 : T a b l e o f l i q u i d l e v e l t o t a n k d i a m e t e r r a t i o s ( J a m e s , 2 0 1 5 ) ....... 81
T a b l e 4 - 1 : M a s s t a r g e t s w h e n s p l i t t i n g ................................................................................ 92
T a b l e 4 - 2 : B o b g e o m e t r i e s .......................................................................................................... 102
Table 4-3: Calculations of shear rate using Estelle et al method and fitting
t h e a n g u l a r s p e e d t o t o r q u e t h r o u g h t h e u s e o f a q u a d r a t i c . ................................ 108
Table 4-4: Table of coefficients of Ω(M) for different orders of polynomial
f i t s f o r S E Q 2 3 3 . ................................................................................................................................. 110
Table 4-5: Comparisons of the derivatives of angular speed with respect to
t o r q u e ( dΩdM) b e t w e e n t h e d i f f e r e n t o r d e r s o f a n g u l a r s p e e d ( Ω ( M ) ) f o r
S E Q 2 3 3 . ................................................................................................................................................... 110
Table 4-6: Comparisons of the shear rates estimated with different orders
of Ω(M) for SEQ233. Some data is excluded as it was found to be in the
T a y l o r r e g i o n . ...................................................................................................................................... 111
Table 4-7: Comparison of the parameters of the Casson curve. The directly
fitted curve refers to the parameters found using the method as described
in section 4.9.4. The fitted to Estelle column refers to the fit as seen in
F i g u r e 4 - 5 . ............................................................................................................................................. 113
Table 5-1: A table showing the correction factors used for calculating
s h e a r s t r e s s ............................................................................................................................................ 119
Table 5-2: Size distribution on as provided material sieved to less than 1
m m ............................................................................................................................................................... 125
Table 5-3: The size distribution of the material after being sieved to less
t h a n 1 m m a n d u n d e r g o i n g a f u r t h e r 5 m i n u t e s o f g r i n d i n g ................................. 127
T a b l e 5 - 4 : N T S 0 4 7 r e s u l t s .......................................................................................................... 128
Table 5-5: Rheology and sedimentation charact eristic parameters measured
a t t h e h i g h e s t s o l i d c o n c e n t r a t i o n a c h i e v e d . .................................................................. 130
Table 5-6: Rheology and sedimentation characteristic parameters measured
a t t h e h i g h e s t s o l i d c o n c e n t r a t i o n a c h i e v e d . .................................................................. 131
T a b l e 6 - 1 : P a r t i c l e s i z e i n f o r m a t i o n f o r t h e g r o u n d s a m p l e s .............................. 147
T a b l e 6 - 2 : C l a y i n f o r m a t i o n ........................................................................................................ 161
Table 7-1: Summary of swelling behaviour amongst the different domains
....................................................................................................................................................................... 179
T a b l e A - 1 : S e q u e n c e l i s t .............................................................................................................. 198
T a b l e B - 1 : N T S 0 3 7 r e s u l t s .......................................................................................................... 214
T a b l e B - 2 : N T S 0 3 8 r e s u l t s .......................................................................................................... 215
T a b l e B - 3 : N T S 0 4 9 r e s u l t s .......................................................................................................... 216
T a b l e B - 4 : N T S 1 0 8 r e s u l t s .......................................................................................................... 217
T a b l e B - 5 : N T S 1 0 8 G r i n d f o r 5 m i n u t e s ............................................................................ 218
T a b l e B - 6 : N T S 1 0 9 ........................................................................................................................... 219
T a b l e B - 7 : N T S 2 3 8 ........................................................................................................................... 220
T a b l e B - 8 : N T S 0 0 8 r e s u l t s .......................................................................................................... 222
xxiii
T a b l e B - 9 : N T S 1 1 1 a s p r o v i d e d r e s u l t s .............................................................................. 224
T a b l e B - 1 0 : N T S 1 1 1 a f t e r g r i n d i n g f o r 5 m i n u t e s ...................................................... 225
Table B-11: Solids concentration and swelling details for NTS111 after
g r i n d i n g f o r 5 m i n u t e s ................................................................................................................... 226
T a b l e B - 1 2 : N T S 2 3 9 r e s u l t s ....................................................................................................... 227
T a b l e B - 1 3 : S o l i d s c o n c e n t r a t i o n a n d s w e l l i n g d e t a i l s f o r N T S 2 3 9 ............... 228
T a b l e B - 1 4 : N T S 0 1 0 r e s u l t s ......................................................................................................... 230
T a b l e B - 1 5 : S o l i d s c o n c e n t r a t i o n a n d s w e l l i n g d e t a i l s f o r N T S 0 1 0 ............... 231
T a b l e B - 1 6 : N T S 1 0 6 r e s u l t s ....................................................................................................... 232
T a b l e B - 1 7 : N T S 1 2 8 r e s u l t s ....................................................................................................... 233
T a b l e B - 1 8 : N T S 0 4 7 r e s u l t s ....................................................................................................... 234
T a b l e B - 1 9 : N T S 1 1 0 r e s u l t s ....................................................................................................... 235
T a b l e B - 2 0 : S o l i d s c o n c e n t r a t i o n a n d s w e l l i n g d e t a i l s f o r N T S 1 1 0 ............... 236
T a b l e B - 2 1 : N T S 1 1 0 a f t e r 5 m i n u t e s g r i n d i n g ............................................................... 237
Table B-22: Solids concentration and swelling details for NTS110 after
f i v e m i n u t e s o f g r i n d i n g ............................................................................................................... 238
T a b l e B - 2 3 : N T S 2 4 0 r e s u l t s ....................................................................................................... 239
T a b l e B - 2 4 : N T S 0 2 7 r e s u l t s ....................................................................................................... 241
T a b l e B - 2 5 : N T S 0 4 4 g r o u n d f o r 5 m i n u t e s r e s u l t s ..................................................... 242
Table B-26: Solids concentration and swelling details for NTS044 after
f i v e m i n u t e s o f g r i n d i n g ............................................................................................................... 243
T a b l e B - 2 7 : N T S 0 4 5 r e s u l t s ....................................................................................................... 244
T a b l e B - 2 8 : N T S 0 4 6 r e s u l t s ....................................................................................................... 245
T a b l e B - 2 9 : S o l i d s c o n c e n t r a t i o n a n d s w e l l i n g d e t a i l s f o r N T S 0 4 6 ............... 246
T a b l e B - 3 0 : N T S 0 5 4 r e s u l t s ....................................................................................................... 248
T a b l e B - 3 1 : N T S 0 5 4 a f t e r g r i n d i n g f o r 5 m i n u t e s r e s u l t s ..................................... 249
Table B-32: Solids concentration and swelling details for NTS054 after 5
m i n u t e s g r i n d i n g ................................................................................................................................ 250
T a b l e B - 3 3 : N T S 1 0 0 r e s u l t s ....................................................................................................... 251
T a b l e B - 3 4 : N T S 0 1 9 r e s u l t s ....................................................................................................... 252
T a b l e B - 3 5 : N T S S 0 5 5 r e s u l t s .................................................................................................... 254
T a b l e B - 3 6 : N T S 0 9 7 r e s u l t s ....................................................................................................... 255
T a b l e B - 3 7 : N T S 0 9 7 a f t e r g r i n d i n g f o r 5 m i n u t e s ...................................................... 256
Table B-38: Solids concentration and swelling details for NTS097 after 5
m i n u t e s g r i n d i n g ................................................................................................................................ 257
Table E-1: Measuring system characteristics of SEQ233. SEQ233 used the
large bob and the RM180 rheometer in the wide gap configuration
d e s c r i b e d e l s e w h e r e i n t h i s t h e s i s . ........................................................................................ 276
T a b l e E - 2 : M e a s u r i n g s y s t e m p r o p e r t i e s ........................................................................... 276
Table E-3 Averaged raw data and the calculat ed shear stress and angular
v e l o c i t y r e s u l t s . ................................................................................................................................. 277
Table E-4: Data used for calculating shear rate. From Table E -3, the last 5
rpm rate is treated as the equilibrium yield stress. At 500 rpm, the torque
exceeded the manufacturers specification, so the data point is omitted from
f u r t h e r a n a l y s i s . ................................................................................................................................. 279
xxiv
Table E-5 : The components required for the Estelle approximation.
H i g h l i g h t e d i n r e d i s t h e p h y s i c a l l y i m p o s s i b l e r e s u l t o f a n e g a t i v e 𝑑𝛺𝑑𝑀.
....................................................................................................................................................................... 284
Table E-6: SEQ233 angular speed vs torque fits. As can be seen they are
split into three parts labelled a, b, and c referring to three separate parts
o f t h e c u r v e s h o w n i n F i g u r e 4 - 3 . .......................................................................................... 285
T a b l e E - 7 : T h e s h e a r r a t e c a l c u l a t i o n u s i n g t h e E s t e l l e m e t h o d . ..................... 286
Table E-8: Calculating the Taylor number with the Estell e method. The red
l i n e s i n d i c a t e c e l l s w i t h T a y l o r v o r t i c e s ........................................................................... 289
T a b l e E - 9 : F i n a l r e s u l t f r o m t h e E s t e l l e c a l c u l a t i o n ................................................ 292
T a b l e E - 1 0 : T h e p a r a m e t e r s o f t h e C a i s s o n f l u i d m o d e l ......................................... 296
T a b l e E - 1 1 : S t e p s 2 a n d 3 o f t h e C a s s o n a n a l y s i s ...................................................... 296
Table E-12: The Taylor number calculation technique. Note, for this
example, the shearing is always partial due to the high yield stress. Under
t h e f u l l y s h e a r e d c o n d i t i o n t h e d i s t a n c e w o u l d b e 0 . 0 1 m .................................... 298
T a b l e E - 1 3 : T h e p a r a m e t e r s o f t h e C a s s o n f l u i d m o d e l ........................................... 299
T a b l e E - 1 4 : S t e p s 2 a n d 3 o f t h e C a s s o n a n a l y s i s ...................................................... 299
T a b l e E - 1 5 : T a y l o r d a t a ................................................................................................................ 300
T a b l e E - 1 6 : F i n a l r e s u l t s o f t h e C a s s o n m e t h o d .......................................................... 301
List of abbreviations
F = correction factor
M = torque
r = radius
r2 = rc or ry
xxv
R = linear correlation coefficient
R2 = coefficient of determination
Ta = Taylor number
γ̇ = shear rate
η = viscosity
ηB = Binghman viscosity
η∞ = infinite viscosity
τ = shear stress
τ0 = yield stress
ϕ = solids concentration
Ω = angular speed
xxvi
Chapter 1
Introduction
1.1 Background
Comminution operations have a high energy intensity. It has been
reported that comminution processes consume approximately 1.8% of
the world’s generated electrical energy; the comminution of gold and
copper ores alone consume about 0.2% (CEEC, 2016). Improving the
efficiency of mills clearly has the potential to reduce the energy cost,
operating cost and environmental impact of a mine. The rheolo gical
characteristics of wet ground ores are known to affect the energy
efficiency, throughput, and total recovery of minerals; it is believed
these effects are significant yet they are still not well understood
(Shi, 1995).
1
Previous research by Klimpel (1984) has found four major factors
that affect slurry rheology:
2. Fines content
3. Slurry temperature
4. Chemical environment
2
1.3 Statement of Sustainability
This research was undertaken whilst studying at the Julius
Kruttschnitt Mineral Research Centre (JKMRC) which is a part of the
University of Queensland’s Sustainable Minerals Institute ( SMI). As
such, the research undertaken was done under the broad goal of
sustainability.
All of these benefits will not involve any new technology, rather,
they stem from improved management. The research allows a better
scientific understanding of ore and how to process it. As such, these
improvements should be rapidly implementable.
3
Chapter 3 explains the commissioning of the rheology
experimental equipment. This includes discussion explaining
rheometer selection, selecting an appropriating coaxial gap, and the
design considerations behind commissioning the “testing rig”
component of the helical flow rheometer. Of the preceding tasks, the
commissioning of the testing rig component of the flow rheometer was
the most important contribution in this chapter. The testing rig is the
component of the flow rheometer which circulates and mixes slurry
preventing it from settling. It consists of several pieces of equipment
that had to be either designed and constructed at the JKMRC pilot
plant or altered to handle slurry flow such as a sump, a pump, a
measuring chamber, a mixing impeller and the associate d piping.
4
Chapter 2
Literature Review
As this project is fundamentally about understanding the
rheology and the stability of Lihir ores, and how the effe cts of the
underlying properties interact, the literature review covers:
1. Kaolinite
2. Illite/Smectite
3. Montmorillonite
5
Figure 2-1: Schematic approximation of variation in Lihir
mineralogy as taken from Gardner (2016). The new domains currently
used by Newcrest may be seen on the lower horizontal axis whilst the
older domain characterisation is on the upper horizontal axis. The y -
axis is the weight percentage (wt%)
6
Table 2-1: The average gold and sulphur content of the Lihir ore
'types'
7
Figure 2-2: Pyrite value classification diagram. No chemical or
textural spatial distinction established. Taken from (Gardner, 2016).
8
most processes and it is only necessary to consider the viscous
effects.
9
As is commonly known there are several types of time
independent flow as shown in Figure 2-3. Under Newtonian flow, the
fluid has a constant viscosity and flow initiates under even very small
forces. A fluid which undergoes shear ind uced thickening (i.e. grows
more viscous the larger the force tha t is applied) is called dilatant
whilst shear induced thinni ng (becomes less viscous when a greater
force is applied) is called pseudoplastic. Examples of these
phenomenon include (but by no means are limited to): water is a
Newtonian fluid, concentrated s and suspensions are dilatant (Barnes,
1989), and polymers are typically pseudoplastic (Rapp, 2017).
10
it contains clay minerals which often display thixotropic effects (see
section 2.9). Tadros (2010) described three types of time dependent
flow:
1. Thixotropic
2. Anti-thixotropic
3. Rheopectic
11
The step change test is where the slurry is subjected to a
constant high shear rate. The application of the shear rate needs to be
sudden, ideally instantaneous. The sheer stress is recorded over a
period of time; eventually the shear stress reaches an equilibrium.
After the equilibrium is reached, the shear rate is suddenly dropped to
a lower value (not zero). The shear stress should suddenly drop and
eventually re-build over time to an equilibrium level of stress
(Tadros, 2010).
12
Figure 2-4: The loop and step tests for determining time -
dependent rheological behaviour. Taken from (Tadros, 2010)
13
w h e r e η(ϕ) i s t h e v i s c o s i t y a s a f u n c t i o n o f t h e p a r t i c l e s v o l u m e
f r a c t i o n , η0 = l i q u i d p h a s e v i s c o s i t y , [η] = t h e i n t r i n s i c v i s c o s i t y ( a
single particle property that depends on factors such as shape and
p o r o s i t y ) a n d ϕ = solids volume fraction. F o r h a r d s p h e r e s , [η]= 2 . 5 , t h e
equation becomes:
𝜂(𝜙)
𝜂𝑟 = = 1 + 2.5𝜙 2-3
𝜂0
w h e r e ηr = relative viscosity. A s t h e e q u a t i o n a s s u m e s n o i n t e r a c t i o n s
between the suspended particles, it only holds when the slurry is
extremely dilute. Numerous authors have expanded the equation as a
power series:
𝜂𝑟 = 1 + 𝑘1 𝜙 + 𝑘2 𝜙 2 + 𝑘3 𝜙 3 + ⋯ 2-4
14
Figure 2-5 : Mendoza (2017) plot of relative viscosity; the
predicted values are represented by the lines and the experimental
values by the symbols
A problem with this work is that they only predict the relative
viscosity (suspension viscosity divided by liquid phase viscosity). As
stated by Shi (1995), in the mineral grinding process, knowledge of
the rheological behaviour of the slurry over a range of shear rates is
more important than knowing the viscosity value of slurry at one shear
rate. The published relationships cannot be used to predict rheological
flow curves of slurry from the measured slurry properties.
15
sphere packing formula and the Quemada (1977) model to analytically
predict the viscosity of a polydisperse su spension of hard spheres.
• solids concentration;
• temperature;
• chemical environment.
16
Figure 2-6: Thixotropy of iron mine tailing slurry (Jeong et al.,
2015)
In addition, it has also been shown that the miner alogy and the
particle shapes also effect rheology (Mueller et al., 2010; Ndlovu,
2014).
18
Figure 2-7: Shi (1995) simulated flow curves of Hellyer grinding
slurry.
19
2.4.2 Particle size distribution
It has been reported that the particle size affects viscosity and
that decreasing particle size increases viscosity (Kawatra, 1988; Shi,
1995). The hypothesis is that decreased particle size increases the
chances for collisions. However, Shi found that some others reported
the opposite; considering that slurry rheology is extremely complex
and is affected by many factors it is possible that secondary effects
overpowered the expected effect of increased viscosity from decreased
particle size. Any tests must control for secondar y effects to be
scientifically accurate. The link between thermodynami c effects and
particle size are negligible at mineral processing sizes.
Shi (1995) believed that a good understanding of the size and the
distribution was key and that the commonly used percent passin g size
was insufficient to describe the particle and size distribution
characteristics. Shi developed a semi-empirical model to predict slurry
rheology which incorporates particle size and distribution; it is
described in section 2.10.1,
20
Figure 2-8: Flow curves of discharge slurries of Emu Gold ball
mills. As can be seen (a) is dilatant with low yield stress whilst (b) is
Pseudoplastic with high yield stress. Taken from Shi (2002).
1) reduce viscosity;
21
3) and reduce the yield point.
22
Figure 2-9: Effect of low molecular weight polyacrylic acid on
the shear yield stress-pH behaviour for a zirconia suspension at 57%
(wt%) (Boger, 2009)
23
Figure 2-10: Zirconia suspension with additive of polyacrylic at
57% with unadjusted pH and 88.7% with adjusted pH (Boger, 2009).
2.4.4 Temperature
Increasing the temperature decreases the apparent viscosity and
the yield point. Often, performing the rheology tests leads to an
increase in temperature which needs to be corrected. Napier-Munn and
Shi corrected temperature by assuming that the changes in the
24
viscosity of the slurry reflect the changes in the eff ect on temperature
(Shi, 1995); a problem with this is that if the viscosity stems from
mechanical interactions between particles the dependence on
temperature may be small.
B i n g h a m : 𝜏 = 𝜏0 + 𝜂𝐵 𝛾̇ 2-5
w h e r e τ i s t h e s h e a r s t r e s s , 𝛾̇ i s t h e s h e a r r a t e , 𝜏0 i s d e f i n e d a s t h e
y i e l d s t r e s s a n d 𝜂𝐵 t h e B i n g h m a n v i s c o s i t y .
H e r s c h e l - B u l k e y : τ = τ0 + Kγ̇ n 2-6
The issue with using these models to descr ibe slurry rheology
was well expressed by Hallbom (2008) who demonstrated that through
the use of different curve fitting function s dramatically different flow
models were developed. The contradictions were a major concern as
the different flow properties lead to completely different engineering
decisions. He suggested the use of the Casson m odel (2.7) or other
similar models within the same family such as given by 2.8:
25
√𝜏 = √𝜏0 + √𝜂∞ . 𝛾̇ 2-7
The disadvantages of parallel plates are that the shear rate varies
across the gap. Hence, an average shear rate must be determined by
varying the gap width. This task is considerably more difficult in non -
Newtonian fluids. Furthermore, sample filling is a non-trivial process
(Anon, 2016).
The cone and plate geometry are similar to the parallel plate
geometry. The fluid is placed between the cone and the plate; the cone
is attached to the rotor. Like the parallel plate geometry, sample
filling the cone and plate is a non-trivial process. Unlike the parallel
plate geometry the shear rate is constant throughout the sample (Anon,
2016).
27
The chief advantage of the cone and plate are that it has a
consistent shear rate throughout the sample (Anon, 2016). They are
also quick and easy to clean (Anon, 2016).
28
As discussed by Krieger and Elrod (1953), the shear rate is
dependent upon the fluid model and may be calculated by:
𝛾̇ = 𝑓(𝜏1 ) 2-9
r γ̇ 1 τ f(τ)
Ω = ∫r 2 r dr = − 2 ∫τ 2 dτ 2-10
1 1 τ
where Ω = angular speed. The shear stress at the surfac e of the bob
is calculated by:
𝑀
𝜏1 = 2𝜋𝑟 2 𝐿 2-11
1
2.6.4 Vane
The vane method is where a spindle is attached to a cylindrical
shaft and lowered into the slurry. It has two variables, shear rate and
29
torque; setting one variable allows the other to be measured. Vane
rheology is most often used for finding the yield stress (Barnes and
Nguyen, 2001).
Nguyen and Boger (1983) introduced the vane method for finding
the yield point to minerals processing from soil science. The vane
method is simple to use, allows the direct measurement of yield stress
and avoids wall slip. The yield point is found by increasing the stress
applied to a system over time. As the yield point is reached the vane
begins to rotate.
30
As written earlier, Shi and Zheng (2003) used a vane geometry to
measure the rheology of a flotation circuit. Shi and Zheng (2003)
argued that vane rheology:
Li et al. (2015) vane and cup system can estimate shear stress by
the equation 2-12.
𝑀 𝑀
𝜏=𝐾 = 𝐿 2 2-12
𝑣 2𝜋𝑟 3 ( + )
𝑟 3
where shear stress (τ), vane constant parameter (K v), torque (M),
radius (R), length of the vane (L). To estimate shear depends if the
material is partially or fully sheared. If partially sheared, the
infinite sea solution could be used (see section 2.7.2) and if fully
sheared a modified Krieger solution (see section 2.7.3). To decide
whether the system is partially or fully sheared:
𝜏
𝑟𝑦 = 𝑟1 . √𝜏 2-13
0
w h e r e t h e s h e a r e d r e g i o n i s 𝑟𝑦 .
31
applied to the reservoir causing it to flow through the capillary tube;
viscosity is determined from the pressure drop and fluid flow rate
(Akroyd, 2004). Previous researchers have found the capillary
(Nguyen and Boger, 1985) to be effective at determining the rheology
of mineral suspensions, however, the capillary rheometer has two
major drawbacks when testing mineral suspensions: it requires a large
amount of sample and a large capillary (Fisher et al., 2007). Due to
particle migration effects, it is not suitable for rapidly settling
slurries (Akroyd, 2004).
2.6.6 Summary
Four geometries of rotational rheometers were discussed in the
previous subsections (2.6.1 through 2.6.4). Upon review, the selection
of the coaxial cylinder geometry was sound as
• the cone and plate geometries are unsuitable for wide gap
geometries;
32
• the parallel plate was more difficult to modify for settling
suspensions;
1. a narrow gap geometry is used, and the wall slip, and non-
Newtonian effects assumed negligible;
33
The Newtonian shear rate is given by
2Ω.𝑟 2
𝛾̇ = 𝑟 2 −𝑟12 2-14
2 1
The standard requires that the size of any solid particles in the
sample shall not be greater than one fifth of the narrowest point in the
measurement gap.
34
Figure 2-16: Coaxial cylinder image taken from ISO (1995)
35
w h e r e a n g u l a r s p e e d ( Ω) , o u t e r r a d i u s ( r2 ) , i n n e r r a d i u s ( r1 ) , s h e a r r a t e
( 𝛾̇ ) , s h e a r s t r e s s ( τ) , s h e a r s t r e s s a t t h e o u t e r r a d i u s ( τ2 ) , s h e a r s t r e s s
a t t h e i n n e r r a d i u s ( τ1 ) , a n d t h e f l u i d m o d e l ( f(τ)) t o b e s o l v e d w i t h o u t
any additional knowledge of the fluid model (Krieger, 1952). As
explained by Nguyen and Boger (1987), the shear rate is given by:
Ω
𝛾̇ = 2 n 2-15
𝑑𝑀
𝑛= 2-16
𝑑𝛺
Ω (𝑚.𝑙𝑛𝜀)2 (𝑙𝑛𝜀)2 𝑑𝑚
𝛾̇ = 𝑙𝑛𝜀 . (1 + 𝑚. 𝑙𝑛𝛼 + + . 𝑑𝑙𝑛(𝜏)) 2-18
3 3
w h e r e s h e a r r a t e ( 𝛾̇ ) , a n g u l a r s p e e d ( Ω) , c u p t o b o b r a d i u s r a t i o
(α), yield stress (τ0) and
𝑑𝑙𝑛Ω
𝑚 = 𝑑𝑙𝑛(𝜏) 2-19
36
alternative shear rate calculations are performed : a fully sheared and a
partially sheared condition.
𝑑Ω
𝛾̇ = 2𝑀 (𝑑𝑀) , 𝑖𝑓 τ2 < τ0 2-20
𝑑Ω 𝑑Ω
𝑀( ) Ω−𝑀( )
𝑑𝑀 𝑑𝑀
𝛾̇ = 2 𝑟2
− 𝑟1 , 𝑖𝑓 τ2 > τ0 2-21
1−( 12 ) ln( )
𝑟2
𝑟2
w h e r e s h e a r r a t e ( 𝛾̇ ) , t o r q u e ( M ) , a n g u l a r s p e e d ( Ω) , y i e l d s t r e s s
( τ 0 ) , o u t e r r a d i u s ( r2 ) , i n n e r r a d i u s ( r1 ) , s h e a r s t r e s s a t t h e o u t e r
r a d i u s ( τ2 ) , s h e a r s t r e s s a t t h e i n n e r r a d i u s ( τ1 ) .
37
coaxial cylinder; another is the use of helical flow rheometers.
38
Figure 2-18: Rheological measurements of a fly ash slurry using
a standard bob and cup geometry (Akroyd, 2004).
39
Newtonian solution produces minimum error by comparing the results
of the Newtonian calculation with the Krieger.
2.8.2 Debex
Debex style rheometers have been used in several projects at the
JKMRC (Reeves, 1990; Shi, 1995, 2016). Slurry is pumped into a
measuring chamber where the viscosity could be measured as a Couette
flow. The pressure head was maintained by the overflow.
40
Figure 2-20: A schematic of a testing rig built on the same
principles as the Debex rheometer (Shi, 2016)
41
and axial effects weren’t considered in the data analysis. Another
acknowledged difficulty was turbulence effects; complica ted
statistical work was conducted to overcome these issues (Shi, 1995).
Furthermore, these rheometers were designed to consu me a large
volume of slurry required (greater than 20L). I was unable to find any
detailed discussion of the commissioning of such rheometers nor their
start-up within the literature.
42
find any discussion in the start-up of the helical flow rheometer.
Akroyd (2004) also faced difficulties with re-circulating his slurry.
43
Figure 2-23 Error in shear rate between flow rheometer data
analysed using helical flow and Couet te flow theory for a 1 wt% CMC
solution (taken from Akroyd (2004))
44
Figure 2-24: Apparent viscosity of quartz and amorph ous silica
suspensions at 100s-1 as a function of solids concentration (Chen et
al., 2017)
2.9.1 Clay
Clays are well known as a complicating factor in mineral
processing caused by numerous properties of clay such as clay
agglomerating and swelling. In additional, clay particles have been
shown to increase the viscosity and the y ield stress (Cruz and Peng,
2016).
45
join together to form particles, which can aggregate into larger
assemblies as shown in Figure 2-25.
46
Figure 2-25: Diagram showing a clay mineral layer (A); a
particle (B); an aggregate (c); and an assembly of aggregates (D)
(taken from Bergaya and Lagaly (2013)).
47
Figure 2-26:edge/face and face/face contacts that link the
particles to a house of cards (a) or a band-like (b) structure (Lagaly,
1989).
48
2.9.2 Lihir Clays
The Lihir domain classification system includes clay and as
stated in section 2.1 consists of kaolinite, illite/smectite, and
montmorillonite. It is likely that, from the most to the least complex
effects on rheology is likely to be (in descending order from the most
complex to the least): smectites (including montmorillonite);
kaolinite; then illite (Farrokhpay et al., 2016; Ndlovu, 2014). The
structure of these clays is given in Figure 2-27.
49
2.9.2.1 Kaolinite
Kaolinite is a 1:1 structure (Bergaya and Lagaly, 2013; Bridges,
2014; Chakraborty, 2013; Cruz et al., 2015). Kaolinite does not swell
due to its fixed 1:1 silicon atom to aluminium atoms held together by
oxygen and has little isomorphic substitution and a low cation
exchange capacity (Bridges, 2014).
50
2.9.2.3 Montmorillonite
Montmorillonite is a variety of smectite. It has a 2:1 layer
structure, a cation exchange capacity and the ability to swell. Smith et
al. (2000) referenced a case where montmorillonite had both
thixotropic and anti-thixotropic depending on the shear rate history.
2.9.2.4 Mixtures of different clays
Merrill et al. (2017) compared the slurry rheology of different
compositions of five minerals; three minerals were clay mine rals (two
bentonites, primarily montmorillonite from different sources and a
kaolin), quartz and white mica. Up to three minerals out of five were
combined allowing the production of ternary plots comparing how
different mineral combinations effect the rh eology. It was found that
blending these ores led to synergistic effects; the rheology was lower
in mixtures then in either components pure state (see Figure 2-28).
Merrill et al. (2017) proposed several theories to explain these effects
such as the changes in the microscopic structure or that the presence
of multiple minerals result in competitive ion adsorption generating
non-DLVO interactions. The knowledge of these synergetic effects
could lead to beneficial decision making including blendin g ores to
reduce yield stress and viscosity.
51
Figure 2-28: Viscosity ternary plots in volumetric fractions at
ph7. Note, that the plots are a different solid concentration ; the solids
are at 15% and 30% volumetric concentration for the graphs on the left
and right respectively.
2.9.2.5 Summary of Lihir clays
It is likely that, from the most to the least complex effects on
rheology is likely to be (in descending order from the most complex to
the least): smectites (including montmorillonite); kaolinite; then illite
(Brandenburg and Lagaly, 1988; Farrokhpay et al., 2016; Ndlovu,
2014). Both smectites and kaolinite are known to display time
dependency (Lagaly, 1989; Smith et al., 2000); this time dependency
is highly complex consisting of both thixotropy and anti -thixotropy.
Both of these models are of limited use in slurries with high clay
contents in regard to flotation performance. The models do not give,
or in fact incorporate, information on particle associations as they are
focused on yield stress and apparent viscosity; metrics which fail to
predict floatation performance in slurries wi th high clay contents
(Cruz and Peng, 2016). This is likely due to time dependent effects
such as thixotropy stemming from the clay particle agglomerates.
53
Figure 2-29: Time dependent viscosity of nuclear waste slurries
showing thixotropic, anti-thixotropic and time independent behaviour
under different shear rates (Smith et al., 2000).
54
materials typically show a yield stress while anti -thixotropic material
are often flowable fluids at low stress that becom e more viscous or
even solid-like during and after flow.
55
behaviour (Brandenburg and Lagaly, 1988; Coussot et al., 2002;
Lagaly, 1989). Coussot et al. (2002) defined these flow curves as
being “viscosity bifurcation”; unlike ideal yield stress fluids they stop
flowing abruptly below a critical stress and start flowing at a hi gh
velocity beyond a critical stress which in addition increase with the
time of preliminary rest. Hence, for such fluids there is no
(homogeneous) steady state flow at a shear rate below a critical value
as there is bifurcation of the behaviour towards ei ther stoppage or
rapid shear. This effect is illustrated in Figure 2-31.
57
2.9.5 Accurate sizing of clay particles
Clay science is a multidisciplinary field in which the scientists
have a wide variety of backgrounds including geology, mineralogy,
chemistry, physics, and biology reflecting the wide variety of interest
in its applications. This has incidentally led to several different
definitions of clay; and while there is no generally agreed upper limit
to the particle size of clay it is a key parameter in all definiti ons
(Bergaya and Lagaly, 2013).
58
smaller than 38 μm and cyclosizing is not appropriate for mixtures
with large differences in particle weights (Napier-Munn et al., 1996).
Care should be taken when comparing the results from different sizing
techniques as seen in Figure 2-33.
60
The advantage of Shi’s MV model, is that it allowed rheology to
be inferred without measurement. This is highly useful when
measurement is physically difficult to perform such as inside a
grinding mill. Its faults were th e inability to translate the results to
other rheometer, it involved complicated data reduction procedures,
and as can be seen involves many parameters.
2.10.1.2 Breakage and mass transport
Slurry rheology affects milling energy efficiency as it influences
both the breakage behaviour and the mass transpo rt mechanism (Shi
and Napier-Munn, 2002). Shi and Napier-Munn (2002) developed a
macroscopic term they named the Grinding index which represented
the overall breakage of particles passing through a grindi ng mill. It is
not based on a size by size breakage rate nor does it take into account
the mill throughput and power consumption and hence, it cannot be
said that increasing grinding index necessarily increases the grinding
efficiency. Despite these limitations, the grinding index allows certain
interpretations on grinding to be developed.
𝑆 −𝑆
𝐷 𝐹
𝐺𝑟𝑖𝑛𝑑𝑖𝑛𝑔 𝐼𝑛𝑑𝑒𝑥 = (100−𝑆 ) ∗ 100 2-25
𝐹
where
61
• If a slurry has a high yield stress further increasing slurry
density will significantly increase the apparent viscosity
and decrease the grinding index.
2.10.2 Flotation
Flotation is a popular separation technique that uses differences
in surface properties to separate valuable minerals from gangue as
shown in Figure 2-34. A ground slurry is diluted and treated with
reagents making either the minerals or the gangue hydrophobic befor e
being fed into the flotation cell. The flotation cell aerates the slurry;
the hydrophobic particles attach to the bubbles surfaces and are
transported to the pulp surface. Froth, three phase bubbles, forms a
zone at the top of the pulp; the froth is tran sported over the
concentrate lauder. Not all of the froth makes it to the concentrate;
some of the bubbles coalescence or burst and the particles they were
carrying return to the pulp zone.
62
Figure 2-34: The flotation process. Taken from Li (2016)
𝑑2 (𝜌𝑠 −𝜌𝑓 )𝑔
𝑈∞ = 2-26
18𝜂
w h e r e 𝑈∞ i s f r e e s e t t l i n g v e l o c i t y , d i s t h e d i a m e t e r o f t h e
settling solid, ρ is the density, g is gravity and the subscripts s and f
refer to solid and fluid respectively. There are several issues with the
use of equation 2-26 in the sedimentation of mineral slurries; of these
three are particularly relevant for this study. Firstly, mineral particles
are neither spherical nor are they of a uniform size. Secondly, mineral
slurries often display yield stress; m aterials with sufficient yield
64
stress (Ovarlez et al., 2012) do not settle. Thirdly, mineral slurries
and suspension have high concentrations; at hig h concentrations of
solids hindered rather than free settling occurs (Lee, 1989).
65
Figure 2-35: Ferrosilicon sedimentation rate at a variety of
densities (Shi, 2016)
66
The clays contained in Lihir are known to swell (see section
2.1). For reliable rheology it is required to know the volume
concentration; however, the point of this project is to apply this
knowledge to a real grinding circuit (see sections 1.1 through 1.3 for
more details). As such the slurries should be well mixed before
beginning the experiments but not mixed for so long that they are not
materially similar to what would be occurring in the grinding circuit.
Swelling, if it occurs, would cause a decrease in the water volume and
an increase in the clay size thus leading to an increase in the solid
volumetric concentration. If this occurs during a rheology experiment,
then the effects of increasing solids concentration will be observed.
67
agree with the sceptics and believe that the material wi ll
not transition from Newtonian to shear thickening to
shear thinning.
68
• how to build and operate a helical flow rheometer allowing
the accurate measurement and production of flow curves for
a coarse unstable slurry with a high clay content and
limited sample;
69
Chapter 3
Testing rig and rheometer
commissioning
At the beginning of this project it was believed by the
supervisory team that the Lihir ore slurry would be fast settling even
at the high concentrations (see section 2.11) as such the project
required the commissioning of a helical flow rheometer. There were
sample availability constraints which prevented the testing of the
sedimentation rate until after the helical flow rheometer was
commissioned. The initial validation experiments were performed on
outer biotite samples which were found to be fast settling. However,
through the course of this project it was discovered that many of the
samples were in fact slow settling, especially at high concentratio ns.
70
provided at the end of this chapter (secti on 3.5) reviewing the
different considerations and also the changes in the experimental plan.
• used online;
• in an industrial environment;
71
2. Maintaining laminar flow: laminar flow must be maintained
to produce true flow curves. Hence, all data with a Taylor
number greater than 41.3 should be excluded (the point
where Taylor vortices begin to occur). This is explained in
more detail in section 3.1.2.
2. A sediment bed builds which the bob can get caught on.
72
unwanted complexity in an already complicated project . To prove that
the correction method is accurate would require performing the tests
with a control.
73
𝜏 = 𝐴 . 𝑀𝑑 3-1
where Md is the applied torque, τ is the shear stre ss, and A is the
g e o m e t r i c f a c t o r . T h e s h e a r r a t e ( 𝛾̇ ) c a n b e g i v e n b y :
𝛾̇ = 𝐵 . 𝛺 3-2
1 . S e l e c t Ω and η
2 . W o r k o u t 𝛾̇ b y 𝛾̇ = 𝑀 . Ω
3 . W o r k o u t τ b y 𝜏 = 𝜂 . 𝛾̇
𝜏
4 . W o r k o u t M d b y 𝑀𝑑 = 𝐴
74
41.3 < 𝑇𝑎 < 400 ∶ 𝑙𝑎𝑚𝑖𝑛𝑎𝑟 𝑓𝑙𝑜𝑤 𝑤𝑖𝑡ℎ 𝑇𝑎𝑦𝑙𝑜𝑟 𝑣𝑜𝑟𝑡𝑖𝑐𝑒𝑠 3-4
75
As seen in Figure 3-1, a new testing rig was built for this
project. It could be placed in an air -conditioned laboratory, and the
jacketed pipe allowed slurry temperature control. Optimisation
immediately begun as seen in Figure 3-2. A new smaller sump was
designed which allowed less sample to be used in line with the limited
availability whilst also making the cooling pipe redundant.
76
Figure 3-2: The current testing rig
77
1. uses less sample;
78
desired, immersion tubes could be attached to t he rheometer as seen in
Figure 3-4.
3.2.2 Pump
The pump had to handle solid and abrasive particles, and ideally
be non-pulsed. Unfortunately, the most suitable pump available to the
project at the JKMRC pilot plant was peristaltic. It prevented
sedimentation and could handle highly viscous samples, yet it pulsed;
as such, an overflow (rather than the underflow) needed to be used as
to maintain a near constant head within the measuring chamber as
possible.
3.2.3 Sump
The sump’s purpose is to collect and hold the slurry, and to
ensure that it is well mixed. Mixer tank design is still largely an art
with rules of thumb for design. There are two major considerations in
sump design:
• a mass balance;
80
Table 3-1 : Table of liquid level to tank diameter ratios (James,
2015)
A final point, to ensure the best mixing the impeller is placed off
centre which reduces the vortex (Couper, 2010). Considering the small
sump size, and that the intention is to agitate slurry baffles were
believed to be inappropriate.
81
rate is vastly different allowing a lower or higher concentration to be
immediately added.
82
At high concentrations the sample became effectively non -
settling; using co-axial cylinder rheology would thus be quicker,
simpler, and use less sample. On the other hand, it would not allow
the generation of data for the fast settling s lurries. On balance, it was
decided to use the Anton Paar.
• 25 mm internal radius;
The Anton Paar was working very well; then, qui te unfortunately
the computer with the rheology software failed. The IT department
advised that its failure was purel y caused by age. The Anton Paar is
second hand and came with the now broken computer. After
investigating and contacting the suppliers, it was determined that
JKMRC was never supplied with the software installation separate to
the computer; and that it was only licenced for a very old version of
the software. The project funding was inadequate to buy an upgrade to
the software, however, the supplier managed through internal contacts
to track down a copy in Germany. The day after a new computer was
set up the power supplier controlling the rheometer failed and there
were no funds available for repairs.
83
No data from the Anton Paar experiments w as recovered from the
computer. The experiments performed were purely proof of concept
and to familiarise myself with the equipment. However, they
demonstrated that the co-axial rheology experiments could be
conducted on the high concentration samples and that it was quicker
and easier than using the testing rig. Thus, when developing the
experimental program for the RM1 80, a choice was presented between
using the testing rig or using the cup developed for the Anton Paar.
This will be discussed in more detail in the next section.
The choice between using the cup or testing rig was resolved
through a simple proof of concept experiment. A sample’s rheology
was measured at a series of concentrations proceeding from a high
concentration to lower concentrations. The high co ncentrations were
slow settling and the rheology was easy to measure. Once
sedimentation became an issue the testing rig was used; the one
significant alteration from previous experiments being that the RM180
was used in place of the HAAKE.
All of the data was either too low for the torque to be measured
or the mixing was turbulent; sometimes both. Hence, the experimental
plan described in section Chapter 4.
The second immediate issue was to deal with the much smaller
range of possible torque readings. A larger bob allows a smaller shear
stress to be measured for the same torque as seen by
𝑀
𝜏1 = 2𝜋𝑟 2 𝐿 2-11
1
84
Hence, by using two different bobs a larger range of materials
could be measured. A larger bob where increased sensitivity was
required (less viscous, less solid samples), and a smaller bob where
fluid instability or exceeding the maximum torque were possible
issues (such as in more viscous or solid materials).
• Statistical variation
85
Before determining whether shear thickening occurs,
sedimentation, drying, experimental error, chemical instability and
instrument effects must be ruled out. There were samples tha t
appeared to have characteristic time dependent shear thickening in
which sedimentation could be ruled out. Furthermore, the pH was
stable, and the error bars between the two curves didn’t overlap.
Drying however, was a possible issue in some of these ear ly proof of
concept experiments. After the proof of concepts were completed, the
drying issue was addressed by ensuring the samples were tightly
covered with foil until required. However, before starting on the
experimental program, the Anton Paar DSR301 b ecame unavailable as
described above.
No control was placed on how long the sample was being mixed.
Several different samples were selected including ar gillic, outer
biotite and distil chlorite to understand how different domains may
behave differently. Sample NTS045 (an outer biotite sampl e) indicated
86
statistically significant levels of time dependent shear thickening. The
ramping procedure described in section 4.8.4 was used eliminating the
possibility of instrument artefacts. The pH was stable, the sample was
slow settling and the slurry density underwent negligible change. This
left no possibility but time dependent shear thickening. The longer the
sample was mixed, the thicker it became. Hence, mixing times were
made consistent. It was expected that the container’s size, shape, and
the volume of sample could also affect the thickness. As such, these
were also standardised as described in section 4.8.1. The previous
results prior to these chambers were also treated as proof of concept.
87
• and experimenting with operating the testing rig.
A wide gap geometry with an elongated cup was used in both the
rheometer designs. Calculations for the flow curves within a wide gap
coaxial cylinder geometry were presented in the literature review (see
section 2.7). Additional information on how it was applied to this
project is provided in section 4.9. The important considerations are:
88
Chapter 4
Experimental methodology
This section provides an overview of the final methodology for
both the flow rheometry conducted with the HAAKE Viscotester IQ
and also the concentric cylinder rheometry with the Mettler RM180.
Both methods had much in common and discussing them in separate
chapters would be highly repetitive. As discussed in section 3.3, a
limited number of tests were able to be performed due to the failure of
the HAAKE rheometer before completing the testing program.
4.2 Materials
Lihir ore was provided by Newcrest. The received sample was
delivered in two-kilogram bags previously crushed and sieved to less
than 3.35 mm. All ore had been previously stored by Newcrest in
89
Brisbane before being transferred to this project. No site work was
conducted, and the samples were of varying ages.
2. de-ionised water;
1. Sieving;
2. Malvern MasterSizer.
90
The dried plus 38 μm particles were sized via the JKMRC
rotatory screens (“Rotap”) following an internal protocol modelled on
AS 3638 – 1993. In the dry sieving procedure, material is placed on a
stack of seven screens which are then vibrated for 10 minutes. As
more than seven size distributions were required, the undersized was
collected and sieved for a further 10 minutes.
91
quantity of ore based off the solids concentration of the test as seen in
section 4.4.1.
For the flow rheology tests, exact volume of slurry being added
to the testing rig couldn’t be full y controlled due to the difficulties
with loading (see section 3.2.4 for more details).
4.4.1 Splitting
The sample was split using a combination of rotatory splitters,
riffle splitters, and spooning. On consultation with the advisory team
the rotatory splitters were preferred as they are les s likely to adjust
the sample size distribution. Riffle splitters were used in conjunction
with the rotatory splitters, to approach the approximate mass for a
concentration (see Table 4-1).
75% 844.25
70% 744.48
65% 655.15
60% 574.70
55% 501.87
• NTS108 (argillic)
All samples were ground for 5 minutes. A split for sizing was
taken.
93
Figure 4-1: Particle size distribution curves of NTS050 after
grinding for a differential amount of time.
94
For the final coaxial cylinder rheology, the slurry was taken
from the measuring beaker, and poured into the measuring cylinder. A
target of 200 mL was chosen to make results easier to compare. Not a ll
sub-samples had a sedimentation test performed as some were clearly
pastes and it would have been impossible to accurately fill the
measuring cylinder.
1. mixing the slurry and loading the slurry into the testing rig
(4.7.1);
95
4. adjusting the slurries concentration through r emoving
slurry and adding water (section 4.7.4;
The other technique was to partially prepare the slurry below the
desired concentration, begin pumping and add sample to the testing
rig. This was highly time consuming, increased the chances of spills,
and could cause the pump to bl ock as a lower concentration results in
a higher sedimentation rate.
96
In hindsight, the difficulty with loading the helical flow
rheometer was due to the very large differences in the slurries
rheologies between different NTS numbers. It is recommended that
before future flow rheometry is conducted that a coaxial cylinder
rheology and sedimentation pro gram be conducted. From those results,
the lowest viscosity slow settling sample concentration should be
selected to be added to the testing rig. The testing pump can then be
started with some water already being inside to prevent it from
overloading with the addition of the slurry.
The flow rate was controlled through adjusting the pump speed
and opening and adjusting the size of the valve openings.
98
4.8.1 Mixing the sample
Time dependency was identified as an issue. As such mixing was
always conducted in a 1 L plastic beaker for 4 minutes using a drill
with an attached paint stirrer. The procedure operated as follows:
2. Add the ore to the beaker in a fume cabinet (to avoid the
dust)
3. Weigh the ore and calculate the required water to reach the
concentration.
99
The bob was lowered into the sample. If required, the cup was
lightly tapped again to re-level the surface disturbed by the bob’s
entry. The sample was allowed to rest for 30 s.
The bob and cup were always cleaned and dried when changing
the concentration or sample. An air-compressor using plant air was
used to ensure that both were completely dry.
100
Figure 4-2:Small bob and large bob used in RM180 rheometer.
The small bob was used for more viscous slurries whilst the large
bob was used for the less viscous slurries. If the large bob was used
on the more viscous slurries, it would overload; if the small bob was
used on the less viscous slurries it would generate too small torque
readings to generate useful data. They had distinct geometries; the
large bob had a large conical section on its upper side to prevent
sediment being caught whilst the small bob kept the classical structure
described in DIN53019-1. The parameters of the bobs are described in
Table 4-2.
101
Table 4-2: Bob geometries
Bob
Small Large
Radius 7 mm 15 mm
Height (excluding 21 mm 45 mm
conical sections)
Radial gap1 18 mm 10 mm
1 Using the cup described in section 3.4; the cup has a radius of 25 mm and its measuring chamber is 15
mm long
102
allowing the equations for concentric cylinders to be used for the
calculation of the yield stress.
103
4.9 Data reduction
As discussed in the previous sections, the experimental tests for
the helical flow rheometer and the coaxial cylinder were l argely
similar. Essentially, the helical flow rheometer is a coaxial cylinder
rheometer with axial flow. The solution to axial flow has been solved
for the Newtonian solution but it’s still an active area of research for
the helical flow rheometer (Alharbi, 2016). As described in the
introduction of this chapter the results for the flow r heology were
treated qualitatively; they were only evaluated ignoring the axial
component.
104
where F is the correction factor. The calibration results for the RM180
are described in Table 5-1 found on page 119.
𝑀
𝜏1 = 2𝜋𝑟 2 𝐿𝐹 4-1
1
The shear rate, unlike the shear stress, depends on the fluid
model. Assuming the wrong fluid model results in error; the error
scales with a wider gap. As stated in the literature review there are
three popular methods for approximately the shear rate:
2. the Krieger
3. the Estelle
105
Krieger (and Elrod) then went on to produce an approximate
solution to the shear rate equation:
Ω (𝑚.𝑙𝑛𝜀)2 (𝑙𝑛𝜀)2 𝑑𝑚
𝛾̇ = 𝑙𝑛𝜀 . (1 + 𝑚. 𝑙𝑛𝛼 + + . 𝑑𝑙𝑛(𝜏)) 2-18
3 3
𝑑Ω 𝑑Ω
𝑀( ) Ω−𝑀( )
𝑑𝑀 𝑑𝑀
𝛾̇ = 2 𝑟 2 − 𝑟1 , 𝑖𝑓 τ2 > τ0 2-21
1−( 12 ) ln( )
𝑟2
𝑟2
is apparently negative for both the quad ratic and cubic fit, hence,
producing a negative shear rate and thus a negative apparent viscosity.
This is clearly implausible; it could be avoided by splitting the graph
into multiple sections, however, no general procedure for this
106
technique could be found and could result in the data processing
becoming subjective.
50
W = 5E+06M2 - 25072M + 32.566
40 R² = 0.9993
W (s-1)
30
20
10
0
0 0.001 0.002 0.003 0.004 0.005 0.006 0.007
M (N.m)
107
Table 4-3: Calculations of shear rate us ing Estelle et al method
and fitting the angular speed to torque through the use of a quadratic.
Shear rate
108
a similar technique. Both techniques narrow the data rang e; it isn’t
obvious either why either would necessarily produce a smooth curve.
𝛾̇ r e s p e c t i v e l y . A t Ω = 0 . 5 2 t h e s h e a r r a t e s f o r t h e 2 n d a n d 3 r d o r d e r f i t s
are negative; hence, the fitting procedure was clearly inappropriate.
dΩ
For the 4th and 5th polynomials is overestimated at Ω=0.52 as the
dM
values are greater than the val ues for Ω=1.05 which is clearly
infeasible; this results in an overestim ate of the shear rate at Ω=0.52.
Both the 6th and 7th polynomials provide similar results and the Ω v M
curves seemed reasonable.
109
Table 4-4: Table of coefficients of Ω(M) for different orders of
polynomial fits for SEQ233.
Coefficients
Order a7 a6 a5 a4 a3 a2 a1 a0
2nd - - - - - 5185976 -27070.9 36.10419
3rd - - - - 25679982 4884793 -25933.4 34.72377
4th - - - -5.4E+11 8.55E+09 -4.5E+07 99272.69 -80.428
5th - - 7.77E+13 -2.1E+12 2.06E+10 -9.1E+07 185715 -143.855
6th - 1.16E+17 -2.8E+15 2.72E+13 -1.4E+11 3.7E+08 -525830 304.8464
7th 1.71E+19 -3.8E+17 3.23E+15 -1.3E+13 2.34E+10 -1176249 -52065.5 49.98781
Order of W(M)
W M t1 2nd 3rd 4th 5th 6th 7th
dW/dM
0.52 0.002431 30.2 -1860.8 -1732.2 2455.9 3174.7 1118.5 1432.7
1.05 0.00267 33.2 618.0 696.5 2325.0 2424.3 2428.0 2369.1
2.09 0.003034 37.8 4397.2 4416.3 3928.7 3760.4 4181.6 4158.2
3.14 0.003244 40.4 6570.7 6564.9 5627.7 5503.8 5640.5 5670.1
4.19 0.003408 42.4 8273.0 8252.5 7257.3 7206.8 7118.0 7159.4
5.24 0.003529 43.9 9526.8 9498.0 8588.7 8596.1 8390.5 8424.2
6.28 0.00364 45.3 10687.6 10653.3 9898.5 9954.1 9691.5 9709.7
7.33 0.00373 46.4 11618.2 11580.7 10989.6 11076.3 10805.2 10808.2
8.38 0.003853 47.9 12894.7 12855.0 12527.3 12642.2 12409.0 12391.7
9.42 0.00393 48.9 13690.0 13650.1 13499.8 13622.5 13437.1 13409.6
10.47 0.004009 49.9 14508.1 14469.0 14504.6 14626.8 14505.1 14470.2
15.71 0.004311 53.6 17641.7 17614.2 18280.3 18326.0 18487.6 18462.5
20.94 0.004575 56.9 20384.2 20378.4 21282.3 21198.1 21482.4 21502.5
26.18 0.004813 59.9 22852.9 22875.9 23536.8 23352.6 23526.2 23576.5
31.42 0.00502 62.5 24995.2 25050.3 25009.5 24822.5 24740.9 24777.9
36.65 0.005235 65.1 27226.5 27322.0 25937.1 25916.9 25546.7 25524.2
41.89 0.005441 67.7 29361.9 29502.7 26128.7 26527.5 26124.9 26044.5
47.12 0.00563 70.1 - - 25606.8 26709.9 26850.9 26818.7
52.36 0.005826 72.5 - - - - - -
110
Table 4-6: Comparisons of the shear rates estimated with
different orders of Ω(M) for SEQ233. Some data is excluded as it was
found to be in the Taylor region.
Order of W(M)
W M t1 2nd 3rd 4th 5th 6th 7th
Shear rate
0.52 0.002431 30.2 -4.3 -3.9 11.9 15.4 5.4 7.0
1.05 0.00267 33.2 4.0 4.2 12.4 12.9 13.0 12.6
2.09 0.003034 37.8 26.7 26.8 23.8 22.8 25.4 25.2
3.14 0.003244 40.4 42.6 42.6 36.5 35.7 36.6 36.8
4.19 0.003408 42.4 56.4 56.2 49.5 49.1 48.5 48.8
5.24 0.003529 43.9 67.2 67.0 60.6 60.7 59.2 59.5
6.28 0.00364 45.3 77.8 77.6 72.1 72.5 70.6 70.7
7.33 0.00373 46.4 86.7 86.4 82.0 82.6 80.6 80.6
8.38 0.003853 47.9 99.4 99.1 96.5 97.4 95.6 95.5
9.42 0.00393 48.9 107.6 107.3 106.1 107.1 105.6 105.4
10.47 0.004009 49.9 116.3 116.0 116.3 117.3 116.3 116.0
15.71 0.004311 53.6 152.1 151.9 157.6 158.0 159.4 159.2
20.94 0.004575 56.9 186.5 186.5 194.7 194.0 196.6 196.8
26.18 0.004813 59.9 220.0 220.2 226.6 224.8 226.5 227.0
31.42 0.00502 62.5 250.9 251.5 251.1 249.2 248.4 248.8
36.65 0.005235 65.1 285.1 286.1 271.6 271.4 267.5 267.2
41.89 0.005441 67.7 319.5 321.0 284.3 288.7 284.3 283.4
47.12 0.00563 70.1 - - 288.3 300.8 302.3 302.0
52.36 0.005826 72.5 - - - - - -
111
Figure 4-4: Comparison between the Casson approximation and
the Estelle method using a 6th order polynomial fit of Ω(M). The data
was from SEQ233.
112
Figure 4-5: Fitting a Casson model to the Estelle approximation
of SEQ233 using a 6th order polynomial fit of Ω(M).
(mPa.s)
(Pa)
113
4.9.3 Turbulence
Rheology must be performed under laminar conditions. For each
shear rate the Taylor number was found using the local apparent
viscosity and checked to see if in range using:
41.3 < 𝑇𝑎 < 400 ∶ 𝑙𝑎𝑚𝑖𝑛𝑎𝑟 𝑓𝑙𝑜𝑤 𝑤𝑖𝑡ℎ 𝑇𝑎𝑦𝑙𝑜𝑟 𝑣𝑜𝑟𝑡𝑖𝑐𝑒𝑠 3-4
I f τ2 = τ0 :
1 τ
Ω = 2η (τ − 4√τ0 τ + 3τ0 + τ0 ln (τ )) 4-3
∞ 0
1
I f τ2 > τ0 , t h e n τ2 = 𝛼2 τ1 , h e n c e
1 1 1
Ω = 2η ( (1 − α2)τ1 − 4(1 − α)√τ0 τ1 + 2τ0 ln(α)) 4-4
∞
114
The R2 value of the predicted angular speed against the actual
can then be found through the use of the excel “CORRELL” function.
Excel solver was used to fit the parameters to minimise the sum of
squares whilst setting the yield stress to be at least 0 but also be
beneath the minimum measured stress. A third and final re quirement
was that the infinity viscosity was set to be greater than 1 mPa.s as
this is the viscosity of the carrying fluid (water).
4. If the Casson fluid was modelled over any data point which
included Taylor numbers, those points were excluded, and
the process was re-iterated from step 2.
115
𝑅√𝑛−2
𝑡= 4-6
√1−𝑅 2
4.10 Summary
Two type of rheological experiments were performed: the HAAKE
experimental procedure i.e. the helical flow rheometer (see section
4.7) and the RM180 experimental procedure i.e. the coaxial cylinder
method (see section 4.8). The HAAKE procedure is presented here to
give future readers an understanding of conducting flow rheometry
tests; the results presented in chapter 5 and discussed in chapters 6
through 7 are based off the RM180 experimental procedure.
116
most of the data. This processed data is presented in
chapter 5 and discussed in chapters 6 and 7.
117
Chapter 5
Test results
This section provides an overview of both the slurry rheology
and stability (i.e. sedimentation and swelling) results. Analysis is
largely left to the following three chapters; the chief exception to this
is section 5.1 which gives an overview of the calibration of the RM180
and the validation of the final testing procedure. As was first
referenced in section 4.1, the samples each have an NTS number whilst
each rheology test is described by a unique SEQ number.
118
Figure 5-1: Calibration of the RM180 using 486 mPa.s Newtonian
oil (prior to correction factors).
It was found that the results from using the two bobs were
largely comperable. Both bobs indicated Newtonian behaviour when
shearing calibration oil as can be seen in Figure 5-1. The calibration
oil was passed its manufacturer reconmended use by date; however,
the oil was found to have a viscosity of 486 mPa.s through using a
recently callibrated HAAKE viscotester IQ. As can be seen in Table
5-1, correction factors for calculating the shear stress were used to
allow the viscosity to be accurately determined by the RM180.
Figure 5-2: NTS100 53% (v/v) Comparison of raw results for the
large bob
120
To validate that the sample was consistent, and that the
rheometer was reliable, a test was performed where slurry was made
on separate days using different subsamples from the same NTS
number. Each slurry underwent identical sample preparation,
rheological conditions and gave near identical answers as can be seen
in Figure 5-3.
121
ore particle sizes beneath 38 μm as it gives similar results to wet
sieving.
122
beginning of the project that we should be investig ating the slurry
under a polydisperse condition as the slurry within the grinding
circuits are likely to be polydisperse. The particle size dis tribution of
outer biotite is presented in Figure 5-5; other similar graphs are
presented in the Appendix D.
123
Table 5-2 summarises the data by provided the cumulative size
fractions at three fine contents (9.86, 38, and 53 µm) and a series of
passing sizes (P20, P50, and P80). The full results are provided in
both tabulated and graphical forms in Appendix D. Table 5-2 shows
that there is a large variation in the ore particle size and particle size
distribution.
124
Table 5-2: Size distribution on as provided mat erial sieved to
less than 1 mm
125
NTS Alteration Percentage passing Passing size (µm)
domain
-9.86 -38 -53 P20 P50 P80
127
5.4 Summary of the rheology and sedimentation
data
This is a summary of the major results. Further data can be found
in the Appendix B, F, and G.
128
Table 5-5 and Table 5-6 show respectively the results for the
highest concentration achieved and the highest concentration achieved
whilst observing sedimentation. From these tables it is clear that
silica breccia, inner biotite and outer biotite settle at a higher
concentrations and are less viscous. It is also clear that there was a
large variance within and between the domains. This will be discussed
further in chapters 6 and 7.
129
Table 5-5: Rheology and sedimentation characteristic parameters
measured at the highest solid concentration achieved.
Domain NTS Sequence Solids pH Apparent Yield Infinite Sedimentation
number (SEQ) volumetric viscosity stress viscosity rate
concentration (mPa.s) (Pa (mPa.s) (mL/hour)
at 50 s-1
Advanced NTS037 158 52 249
Argillic 1.38 2.6 73 NA
Argillic NTS038 394 53 1.83 7192 168.5 716 NA
NTS049 215 53 2.91 1727 46.6 122 NA
NTS108 231 46 2.26 1795 40.5 193 NA
NTS108 247 42 3.17 3364 NA
grind 91.5 232
NTS109 399 53% 2.14 9889 265.9 703 NA
NTS238 293 46% 2.17 1804 49.7 120 NA
Upper NTS008 193 53% 6.51 2160 61.903 127.54 NA
epithermal NTS111 346 58% 1.96 2838 115.1 28 NA
NTS111 3014 NA
grind 180 53% 2.24 96.8 119
NTS239 361 53% 4.04 3190 60.6 470 NA
Silica NTS010 351 53% 2.02 842 24.4 48.19 0
breccia NTS106 338 53% 2.74 892 27.0 44 0.9
NTS128 263 53% 5.76 510 15.7 24 2.2
Lower NTS047 329 53% 2.9 3902 110.2 241 NA
epithermal NTS110 305 46% 3.43 4792 109.9 499 NA
NTS110 4406
grind 298 41% 4.75 122.1 288 NA
NTS240 289 59% 2.95 3900 138.9 95 NA
Outer NTS027 384 53% 7.3 451 5.9 108.11 2.0
biotite NTS044 1449 NA
ground 270 46% 6.05 44.3 69.16
NTS045 377 53% 5.27 2078 47.9 214.2 NA
NTS046 245 53% 5.57 4728 139.9 251.84 NA
NTS054 375 57% 5.8 1852 44.3 176 NA
NTS054 NA
grind 323 53% 6.00 3313 97.8 178
NTS100 203 53% 6.77 682 10.2 140 1.8
Inner NTS019 374 53% 6.92 539 12.0 59.43 9
biotite NTS055 278 53% 6.42 515 3.4 211 4.0
NTS097 238 53% 4.21 1637 35.9 186 NA
NTS097 NA
grind 313 46% 5.1 1514 40.7 108
130
Table 5-6: Rheology and sedimentation characteristic parameters
measured at the highest solid concentration achieved.
Domain NTS Sequence Solids pH Apparent Yield Infinite Sedimentation
number (SEQ) volumetric viscosity stress viscosity rate
concentration (mPa.s) (mPa.s) (mL/hour)
at 50 s-1
Advanced NTS037 123
Argillic 168 46% 1.33 0.0 123 1.8
Argillic NTS038 389 31% 2.03 7 5 2.6 2 2.7
NTS049 216 46% 2.75 5 1 8 10.8 65 0.5
NTS108 235 36% 2.31 2 1 9 6.7 11 1.2
NTS108 1.1
grind 251 27% 3.22 104 3.4 4
NTS109 397 36% 2.24 318 10.3 12 1.1
NTS238 297 42% 2.26 1076 37.3 30 0.8
Upper NTS008 196 41% 2.64 168 4.152 14.82 1.5
epithermal NTS111 341 53% 2 784 22.5 46 0.3
NTS111 1.7
grind 183 41% 2.31 99 2.7 7
NTS239 356 41% 4.06 368 10.4 23 0.8
Silica NTS010 352 46% 2.03 322 6.5 43.53 0.8
breccia NTS106 338 53% 2.74 892 27.0 44 0.9
NTS128 263 53% 5.76 510 15.7 24 2.2
Lower NTS047 332 46% 2.91 1059 30.0 64 0.2
epithermal NTS110 307 31% 3.39 181 6.0 6 0.8
NTS110
grind 300 31% 4.57 4 9 4 19.0 7 1.3
NTS240 284 51% 2.91 6 1 7 16.5 45 0.8
Outer NTS027 384 53% 7.3 4 5 1 5.9 108.11 2.0
biotite NTS044 0.81
ground 269 42% 5.94 726 25.5 19.20
NTS045 379 46% 5.39 705 13.8 98.8 2.6
NTS046 258 41% 3.86 317 9.0 19.36 0.25
NTS054 364 53% 5.47 828 18.5 91 1.8
NTS054 0.8
grind 324 46% 6.04 815 22.6 53
NTS100 203 53% 6.77 682 10.2 140 1.8
Inner NTS019 374 53% 6.92 539 12.0 59.43 9
biotite NTS055 278 53% 6.42 515 3.4 211 4.0
NTS097 239 46% 4.21 461 13.0 29 1.6
NTS097 5.3
grind 311 38% 5.09 2 2 2 7.0 9
The differences between the maximum solid concentration found
in
131
Table 5-5 was due to the largest differences in viscosities.
Certain samples it was not possible to go to a higher concentration;
for example, NTS110 after 5 minutes of grinding was so solid that it
could maintain its own structure at 46% solid s as seen in Figure 5-6.
Clearly it had become a thick paste and was no longer a slurry.
132
• Appendix A connects the sequence list to the NTS### and
its solid concentration;
133
Chapter 6
Analysis of the slurry
rheology
As seen in chapter 5, several different samples were tested at a
variety of different concentrations. The difference in the results was
dramatic; many samples failed to produce flow curves whilst other
samples were essentially pastes.
134
Figure 6-1: NTS054 at 57% solid volumetric concentration.
135
Figure 6-2 shows the flow curve of a highly time dependent
sample. The area under the ramp down curve is twice the size of the
area under the ramp up. This time dependent shear thickening makes
the analysis highly difficult; shear rate is dependent on the change in
angular speed with regards to shear stress as seen in
r γ̇ 1 τ f(τ)
Ω = ∫r 2 r dr = − 2 ∫τ 2 dτ 2-10
1 1 τ
For the data reduction, the shear rate was fo und for the ramp up
using a similar method to Estellé et al. (2008); the shear rate was then
linked with RPM for the ramp down. This simplified the comparisons,
however, using a relevant time dependent model may yield a more
accurate evaluation of the shear rate. This isn’t a simple task and it is
not clear which time dependent model would be appropriate. As such,
it is likely that the fluid is even more viscous; this is an area
requiring future work. The raw data illustrates the scale of time
dependency as shown by Figure 6-3 and Figure 6-4.
136
Figure 6-4: The raw data of NTS108 (SEQ231) at a solid
concentration of 46% (v/v) being sheared by the small bob at 999
rotations per minute.
137
Figure 6-5:The change in the “yield stress” of an argillic sample
(NTS109 at 53% concentration; SEQ400) prior to the first, second, and
third loop test.
138
6.1.1 Advanced argillic
Only one advanced argillic sample was experimented on: NTS037.
It was displayed no time dependency in any loop tests. Repeats using
the same sample were performed and the viscosity underwent no
change. The pH was extremely low: 1.38 which may have dispersed the
slurry.
6.1.2 Argillic
The argillic clay samples displayed anti -thixotropic, thixotropic
and time independent properties. There were five different argillic
samples NTS038, NTS049, NTS108 (both as provided and ground),
NTS109, and NTS238; each samp le had rather different particle sizes
and particle size distributions. With the exception of NT S049, all
samples were anti-thixotropic at the highest concentration (the exact
concentration varied due to the highly thick nature of the slurry); the
second highest concentration (46%) of NTS049 thickened with time
like the other samples. The size of the anti-thixotropy becomes
smaller as the concentration drops; transitioning to time independent
(noted in every sample) and in NTS108 (as provided) becoming
thixotropic (thins by 17%) at 31% concentration. This thixotropic
behaviour at 31% in NTS108 may hav e been due to sedimentation as
the ground NTS108 was time independent at similar concentrations
(30% and 27%). The sedimentation rate was however low (3.4
mL/hour) and the unground material was significantly more acidic (pH
2.26-2.35 vs 3.17 to 3.22); as discussed in section 6.1.4 this may be a
genuine effect caused by the change in the pH.
139
became time independent and NTS111 (both as provided and ground)
became thixotropic. NTS111 (as provided) was also tested at a higher
concentration of 58%; it was even more thixotropic than at 53%
concentration. NTS111(after grinding) was investigated as shown in
Figure 6-6; the material was clearly anti -thixotropic.
141
independent characteristics of the lower epithermal samples, there was
a great degree of variance in the time dependence within the lower
epithermal samples. For NTS110 it was anti-thixotropic between 46%
and 36% (v/v); the higher the concentration the gre ater the effect. At
these concentrations NTS110 was non -settling; clearly the anti-
thixotropy was dependent on changes in the suspensions structure
rather than an artefact of the device. At lower solid concentrations,
31% and 27% (v/v), the sample transiti oned to become time
independent and thixotropic respectfully. However, this coincided with
the onset of sedimentation so the thixotropy could possibl y be an
artefact of the device (Klein et al., 1995).
142
From analysing NTS097 (after grinding) it appears that inner
biotite is anti-thixotropic at elevated concentrations; the time
dependency becomes less significant as the concentration decreases.
143
6.2 Solids concentration effect on yield stress and
viscosity
Higher solids concentrations, as expected, resulted in an
increased yield stress and apparent viscosity across all tested samples;
Figure 6-7 is a diagram demonstrating the effect of an increase in
concentration on viscosity. Similar diagrams are displayed overlapped
with other samples that share a domain in section 6.4.
144
Figure 6-8: Flow curves of NTS008 (upper epithermal) at 53%
and 46% solids concentration (v/v).
The effect is similar for the apparent yi eld stress. Every “ramp
up” curve in this thesis was well described by the Casson model (see
section 5.4) with the exception of NTS037 at 46% (v/v) which was
Newtonian. This indicates that the concentrations used in this study
remain beneath the critical concentration to cause time independent
shear thickening (Barnes, 1989; Bender and Wagner, 1996; Bertrand et
al., 2002; Hoffman, 1998; Maranzano and Wagner, 2001; Wagner and
Brady, 2009). Barnes (1989) argues that any suspension will
experience shear thickening at a high enough shear rate; Shi and
Napier-Munn (1999) estimated that the shear rate within a ball mill
ranged between 13 and 730 s-1 which is above the highest shear range
achieved in this study. Taking this upper limit into consideration, it is
possible that the suspensions could be shear thickening under the
conditions inside the ball mill. However, Shi and Napier-Munn (1999)
calculated this upper limit from the shear stress applied to a ball
being 110 Pa, assuming a viscosity and that the fluid underwent
145
Newtonian flow. The viscosities of the suspensions investigated in
this study are much higher and are non -Newtonian, as such, it is
unlikely that any sample at the concentrations investigated in this
study would be shear thickening at the shear rates within the ball mill.
This requires further investigation.
146
Table 6-1: Particle size information for the ground samples
Lower 23 36 41 7 99 437
NTS110 Epithermal
147
Figure 6-9: The grinding effect on the relationship of slurry
viscosity with solid volumetric concentration for outer biotite
(NTS054)
148
Figure 6-10: The grinding effect on the relationship of slurry
viscosity with solid volumetric concentration for inner biotite
(NTS097)
149
Figure 6-11: The grinding effect on the relation ship of slurry
viscosity with solid volumetric concentration for argillic (NTS108)
150
Figure 6-12: The grinding effect on the relationship of slurry
viscosity with solid volumetric concentration f or lower epithermal
NTS110
151
Figure 6-13: The grinding effect on the relationship of slurry
viscosity with solid volumetric concentration for upper epithermal
(NTS111)
Shi and Napier Munn (1999), estimated that the shear rate inside
a ball mill ranged between 13 and 730 s -1. The upper limit was
estimated from calculating a shear stress and then, ass uming a
particular apparent viscosity, working backwards to find the shear
rate. The shear stress they calculated was 110 Pa; several of the flow
curves generated as a part of this project had yield stresses within this
range. Such a slurry would not flow as a liquid but rather move as a
solid; this requires further investigation but may be the reason behind
the slurry pooling.
152
6.4 Domain
As discussed in section 2.1, the ore is characterised by Newcrest
into nine domains. Eight of these domains are processed by the mill;
unfortunately, due to sample limitations only seven of these domains
were investigated and diagrams comparing different samples can be
seen below in Figure 6-14 through Figure 6-20. At Lihir SAG
operations operate at solid concentrations ranging from 70 -75% (wt%),
and ball mill at around 70% (wt%); this corresponds to 46 -53% (v/v)
(Shi, 2017b).
153
other sample tested displayed a lack of yield stress. It was also
extremely acidic with a pH of 1.32.
154
Figure 6-16: Apparent viscosity (at a shear rate of 50 s -1) in
relation to solid volumetric concentration for upper epitherma l
samples
155
Figure 6-17: Apparent viscosity (at a shear rate of 50 s-1) in
relation to solid volumetric concentration for silica breccia samples
157
Figure 6-20: Apparent viscosity (at a shear rate of 50 s -1) in
relation to solid volumetric concentration for outer biotite samples
The effect that alteration domain is best seen in Figure 6-21. The
figure compares the various as provided samples at 46% solids
concentration; as is clearly seen certain domains have a larger
apparent viscosity than others but there is significant variance within
each domain. It was not deduced why the Lower Epithermal domain
had such a large outlier. This concentration is at the upper range of
what is used in the SAG mill at the concentration used within the ball
mill (Shi, 2017b).
158
Figure 6-21: Slurry viscosities of various samples at a constant
46% solid volumetric concentration.
159
critical solid’s concentration for each domain all owing the operator
which to keep the slurry beneath. However, as can be seen in Figure
6-14 through Figure 6-20 there was large variance within each domain
thus preventing the recommendation of such a solids concentration.
Additional research is necessary before a critical concentration can be
recommended; in particular future research should establish:
160
Table 6-2:Clay information
Clay information
NTS Alteration domain
QXRD_ClayMica QXRD_ClaySmectite QXRD_ClayChlorite QXRD_ClayKaolinite QXRD_ClayVermiculite QXRD_ClayCorrensite
NTS008 Upper epithermal trace
NTS010 Silica Breccia minor
NTS019 Inner biotite major minor
NTS027 Outer biotite abundant major minor major
NTS037 Advanced Argillic minor minor
NTS038 Argillic minor minor
NTS044 Outer biotite minor minor minor
NTS045 Outer biotite minor trace minor
NTS046 Outer biotite minor minor minor
NTS047 Lower epithermal minor minor
NTS049 Argillic minor minor minor minor
NTS054 Outer biotite minor minor minor
NTS055 Inner biotite minor trace trace
NTS097 Inner biotite major minor minor
NTS100 Outer biotite major minor minor
NTS106 Silica Breccia minor trace
NTS108 Argillic minor major abundant
NTS109 Argillic trace trace trace
NTS110 Lower epithermal minor minor major minor
NTS111 Upper epithermal minor minor
NTS128 Silica Breccia major minor
NTS238 Argillic major minor abundant
NTS239 Upper epithermal minor trace minor
NTS240 Lower epithermal abundant minor
161
This does not mean that there is no dependenc e on clay content.
The pH, particle size and particl e size distribution were all variable.
Rheology is a physical chemistry discipline; and it is well known that
rheology of slurries is often dependent on the chemical environment
(see section 2.4.3). In this project there was no control on the pH of
the slurries; it was merely monitored. The pH varied widely between
the samples, though, observing it in isolation it does not appear to
have affected the rheology as can be seen by Figure 6-22.
162
6.6 Multilinear regression
Due to the complicated nature of the response it was decided to
perform a multilinear regression analysis in order to link the
regression to:
2. the pH;
163
Figure 6-23: Minitab graph of the multilinear regression results
against the fitted values
164
Emeritus Prof. Napier-Munn assisted with the regression analysis
and suggested using the natural log of the apparent viscosity at 50 s -1.
It greatly improved the regression results as seen in Figure 6-25 and
Figure 6-26.
165
Figure 6-26: Minitab’s four in one chart showing the residuals
relationship with the logarithm of the apparent viscosity.
166
The fitted equation of the viscosity logarithm was:
167
Figure 6-27: Surface plot of the logarithm of apparent viscosity
at 50s-1 vs concentration and pH.
168
Figure 6-28: Surface plot of the logarithm of viscosit y at 50 s-1
vs the particle sizes smaller than 9.86 µm and the amorphous silica
content.
169
Figure 6-30: Surface plot of the logarithm of viscosity at 50 s -1
vs the particle sizes smaller than 9.86 µm and the pH
170
Figure 6-31: Surface plot of the logarithm of viscosity at 50 s -1
vs the Kaolinite content and the pH
Further work is possible and needed in this area. The fitted graph
of the logarithm of viscosity shows sta tistical significance and a high
R2 value when made dependent on the aforementioned variables. More
work could be performed varying the particle size distribution
variables (i.e. taking other values than -9.86, -38, -53 µm) and
selecting alternative geological components. In addition, alternative
rheological parameters could, and should, be investigated including
the yield stress and apparent viscosities at different shear r ates.
171
particle size and the pH to allow the mineralogy to be explored with
greater precision.
6.7 Summary
It was hypothesised that concentration and part icle size would
increase the apparent viscosity and yield stress. These hypothesises
were correct as seen in sections 6.2, 6.3 and 6.6; an additional
unexpected effect was that concentration was linked to time
dependency (see section 6.1). A recommended maximum soli ds
concentration cannot be made because the high viscosity and yield
stresses occur at vastly different concentration for different samples
(see section 6.4). Currently, all that can be recomm ended is that the
solids concentration be reduced immediately by adding water if
undesirable rheological behaviour is observed. It is clear that
(ignoring the time dependency) the suspensions at each concentration
studied were plastic and well described by the Casson model. As such,
if a suitable chemical dispersant can be found the viscosity of the
problematic samples can be greatly reduced.
It was also been shown that there is a link between the rheology
and the geology. As can be clearly seen in section 6.4 certain samples
(particularly argillic and lower epithermal) are substantially more
viscous than other samples. However, this study found no clear culprit
for the rheological problems in the QXRD results. A multilinear
regression found that there was a link between the minerology and the
rheology, but it was complicated as it was linked with the logarithm of
viscosity rather than directly with the viscosity itself, and the
mineralogy heavily interacted with the particle size an d the pH.
Neither the particle size nor pH was standardised in this study; this
study was more interested on the rheology of the slurry depended on
the ore as it was provided rather than how it would have been if it had
been altered. This is because at site they currently do not use any
grinding aids and the goal of this study was to understand what the
problems currently are. Certain samples are naturally finer, and their
172
pH’s varied from being extremely acidic to mildly bas ic. The particle
size of certain samples was varied by grinding and found that this
always increased the viscosity, but it was ground for a set amount of
time rather than aiming for a particular particle size. Future
experimental work should control for par ticle size, particle size
distribution and pH as this may reveal more clearly what in the
mineralogy is affected the rheology.
173
Chapter 7
Analysis of slurry stability
The sedimentation rate was predicted to, and was found, to
depend on the solids concentration, the alteration domain, and the
particle size. In addition, it was found that some sedimentation tests
had a time delay before sedimentation began.
174
ease interpretation. This was seen in all of the samples. As discussed
in section 2.11, this could be due to either the increase in yield stress,
viscosity or hindered settling or a combination of the three.
175
rheology of the samples at a low concentration of 20% (v/v) and more
sedimentation data be developed.
177
7.4 Swelling
178
Table 7-1: Summary of swelling behaviour amongst the different
domains
179
7.5 Sedimentation rate and time delay
Several samples experience a time delay in the sedimentation.
This is an interesting observation , considering that some of the
samples which demonstrated this effect had very low torque readings
indicating a small viscosity. NTS008 at 55% showed, as can be clearly
seen in Figure 7-5, a large time delay before sedimentation occurre d;
however, the RM180 was incapable of generating reliable flow curves
on this sample. Further work is required to investigate this
relationship using more precise rheological devices; for this work I
offer the hypothesise that the time delay was caused by a high yield
stress. This effect was not noticed in the previous rheological studies
conducted in the previous studies conducted at the University of
Queensland’s experimental mine site (Shi, 2016).
180
There is a clear delay in the sedimentation where the mudline
drops by 2mL over the first 12 minutes, and then drops another 8 mL
over the next 12 minutes.
• Swelling samples
• Non-settling samples
181
Figure 7-7: Slurry viscosity in relation to sedimentation rate for
the entire ore samples
182
Figure 7-8: Linear regression on the data of slurry viscosity in
relation to sedimentation rate for the entire ore samples
Both Figure 7-7 and Figure 7-8 show the entire ore body rather
than any particular domain. Figure 7-8 indicates a possible proxy
model for viscosity and sedimentation rate. There was lar ge variance
not just between the domains but also within the domains. Further test
work should be performed at low concentrations using a helical flow
rheometer to generate extra data.
183
Despite the need for further experimental work additional
analysis can be performed. It is known that sedimentation and the
viscosity are strongly linked with yield stress (sections 2.2.1, 2.5,
and 2.11), the concentration (sections 6.2 and 7.1) and the particle
size (sections 6.3 and 7.3). It also is not clear what shear rate should
be chosen as the representative for evaluating the apparent viscosity.
Apparent viscosities at other shear rates should be investigated; the
apparent viscosity at a shear rate of 50 s -1 was selected more due to
the limitations of the rheometer not being able to accurately determine
the shear stress for low viscosity tests.
184
Chapter 8
Conclusion and further
work
This chapter provides a summary of the research findings, the
contributions to knowledge and makes recommendations for future
work.
Despite the reduced results from the testing rig, experience with
its design and operation have been acquired. It has been found that:
185
In the case of Lihir ore slurry three phases of the
suspension were observed (with increasing concentration):
186
additional 12 results of duplicated tests are presented on re -used
samples. The major findings are summarised below:
187
kaolinite or amorphous silicates grades. This does not mean
that there was no dependence; future work will be required
to investigate this further.
188
controlled in this experimental program, the effect of pH
on slurry rheology and sedimentation is not conclusive.
189
size distribution and that the exact effects may only be
revealed after further experiments in which these factors
are controlled.
To build this model further test work using the techniques used
in this thesis will need to be conducted:
190
Other validation work:
192
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196
Appendixes Overview
• Appendix A connects the sequence list to the NTS###,
whether it used the large or small bob and its solid
concentration;
197
Appendix A
Sequence list
The sequence list is provided below. The tables in Appendix F
and Appendix G are in the sequence order.
Solid Solid
Advanced
158 Argillic NTS037 Large 74.8% 52.3%
Advanced
159 Argillic NTS037 Large 74.8% 52.3%
Advanced
160 Argillic NTS037 Large 74.8% 52.3%
Advanced
168 Argillic NTS037 Large 70.0% 46.4%
Advanced
170 Argillic NTS037 Large 62.0% 37.7%
NTS111
after 5
minutes
Upper of
180 epithermal grinding Small 75.0% 52.6%
Upper NTS111
181 epithermal after 5 Small 70.0% 46.4%
198
Solid Solid
NTS111
after 5
minutes
Upper of
182 epithermal grinding Large 70.0% 46.4%
NTS111
after 5
minutes
Upper of
183 epithermal grinding Large 65.0% 40.8%
NTS111
after 5
minutes
Upper of
185 epithermal grinding Large 60.0% 35.7%
NTS111
after 5
minutes
Upper of
187 epithermal grinding Large 55.0% 31.2%
NTS111
after 5
Upper minutes
189 epithermal of Large 70.0% 46.4%
199
Solid Solid
Upper
193 epithermal NTS008 Small 75.0% 52.6%
Upper
195 epithermal NTS008 Large 70.0% 46.4%
Upper
196 epithermal NTS008 Large 65.0% 40.7%
Upper
197 epithermal NTS008 Large 60.0% 35.7%
Upper
198 epithermal NTS008 Large 55.0% 31.2%
Outer
203 biotite NTS100 Large 75.0% 52.6%
Outer
204 biotite NTS100 Large 75.0% 52.6%
Outer
205 biotite NTS100 Large 70.0% 46.4%
Outer
211 biotite NTS100 Large 65.0% 40.8%
200
Solid Solid
Outer
224 biotite NTS054 Small 74.9% 52.4%
Outer
225 biotite NTS054 Large 70.0% 46.4%
Outer
226 biotite NTS054 Large 65.0% 40.8%
Outer
227 biotite NTS054 Large 59.9% 35.6%
Outer
228 biotite NTS054 Large 55.0% 31.2%
NTS108
after
additional
4 minutes
236 Argillic of mixing Large 54.9% 31.0%
201
Solid Solid
Inner
239 biotite NTS097 Large 69.9% 46.2%
Inner
240 biotite NTS097 Large 65.0% 40.7%
Inner
241 biotite NTS097 Large 59.0% 34.8%
Inner
243 biotite NTS097 Large 55.0% 31.2%
Outer
245 biotite NTS046 Small 75.0% 52.6%
NTS108
after 5
minutes
of
247 Argillic grinding Small 65.9% 41.8%
NTS108
after 5
minutes
of
248 Argillic grinding Small 62.0% 37.7%
NTS108
after 5
minutes
of
249 Argillic grinding Large 58.0% 33.8%
202
Solid Solid
NTS108
after 5
minutes
of
250 Argillic grinding Large 54.0% 30.3%
NTS108
after 5
minutes
of
251 Argillic grinding Large 50.0% 27.0%
NTS108
after 5
minutes
of
Na Argillic grinding Na 39.0% 19.1%
Outer
257 biotite NTS046 Small 70.0% 46.4%
Outer
258 biotite NTS046 Large 65.0% 40.8%
Outer
259 biotite NTS046 Large 60.0% 35.7%
Outer
260 biotite NTS046 Large 55.0% 31.2%
Silica
263 Breccia NTS128 Small 75.0% 52.6%
203
Solid Solid
Silica
267 Breccia NTS128 Large 65.0% 40.8%
NTS044
after 5
minutes
Outer of
269 biotite grinding Large 66.0% 41.8%
NTS044
after 5
minutes
Outer of
270 biotite grinding Small 70.0% 46.4%
NTS044
after 5
minutes
Outer of
271 biotite grinding Large 62.0% 37.7%
NTS044
after 5
minutes
Outer of
272 biotite grinding Large 58.0% 33.8%
NTS044
after 5
Outer minutes
273 biotite of Large 51.3% 28.0%
204
Solid Solid
Inner
278 biotite NTS055 Large 75.0% 52.6%
Inner
279 biotite NTS055 Large 69.4% 45.6%
Inner
281 biotite NTS055 Large 65.0% 40.8%
Lower
284 Epithermal NTS240 Small 73.5% 50.7%
Lower
288 Epithermal NTS240 Large 69.4% 45.6%
Lower
289 Epithermal NTS240 Small 79.8% 59.4%
Lower NTS110 5
298 Epithermal min Small 65.0% 40.8%
Lower NTS110 5
299 Epithermal min Small 60.0% 35.7%
Lower NTS110 5
300 Epithermal min Large 55.0% 31.2%
205
Solid Solid
Lower NTS110 5
301 Epithermal min Large 50.0% 27.0%
Lower NTS110 5
302 Epithermal min Large 45.0% 23.3%
Lower
304 Epithermal NTS110 Small 65.0% 40.8%
Lower
305 Epithermal NTS110 Small 70.0% 46.4%
Lower
306 Epithermal NTS110 Large 60.0% 35.7%
Lower
307 Epithermal NTS110 Large 55.0% 31.2%
Lower
308 Epithermal NTS110 Large 49.5% 26.6%
NTS097
after 5
minutes
Inner of
310 biotite grinding Large 66.0% 41.8%
NTS097
after 5
minutes
Inner of
311 biotite grinding Large 62.0% 37.7%
206
Solid Solid
NTS097
after 5
minutes
Inner of
313 biotite grinding Small 70.0% 46.4%
NTS097
after 5
minutes
Inner of
317 biotite grinding Large 54.0% 30.3%
NTS054
after 5
minutes
Outer of
319 biotite grinding Large 66.0% 41.8%
NTS054
after 5
minutes
Outer of
320 biotite grinding Large 62.0% 37.6%
NTS054
Outer after 5
321 biotite minutes Large 56.6% 32.6%
207
Solid Solid
NTS054
after 5
minutes
Outer of
323 biotite grinding Small 75.0% 52.6%
NTS054
after 5
minutes
Outer of
324 biotite grinding Small 70.0% 46.4%
NTS054
after 5
minutes
Outer of
325 biotite grinding Large 70.0% 46.4%
Lower
329 Epithermal NTS047 Small 75.0% 52.6%
Lower
332 Epithermal NTS047 Small 70.0% 46.4%
Lower
333 Epithermal NTS047 Large 65.0% 40.8%
Lower
334 Epithermal NTS047 Large 60.0% 35.7%
208
Solid Solid
Silica
338 Breccia NTS106 Small 75.0% 52.6%
Silica
339 Breccia NTS106 Large 70.0% 46.4%
Silica
340 Breccia NTS106 Large 65.0% 40.8%
Upper
341 epithermal NTS111 Small 75.0% 52.6%
Upper
342 epithermal NTS111 Large 70.0% 46.4%
Upper
343 epithermal NTS111 Large 65.0% 40.8%
Upper
345 epithermal NTS111 Large 60.0% 35.7%
Upper
346 epithermal NTS111 Small 78.7% 57.8%
Silica
351 Breccia NTS010 Small 75.0% 52.6%
Silica
352 Breccia NTS010 Large 70.0% 46.4%
Silica
353 Breccia NTS010 Large 65.0% 40.8%
Silica
354 Breccia NTS010 Large 60.0% 35.7%
209
Solid Solid
Upper
355 epithermal NTS239 Small 70.0% 46.4%
Upper
356 epithermal NTS239 Large 65.0% 40.8%
Upper
357 epithermal NTS239 Large 60.0% 35.7%
Upper
358 epithermal NTS239 Large 55.0% 31.2%
Upper
361 epithermal NTS239 Small 75.0% 52.6%
Outer
364 biotite NTS054 Small 75.0% 52.6%
Outer
366 biotite NTS054 Large 70.0% 46.4%
Outer
367 biotite NTS054 Large 65.0% 40.8%
Outer
368 biotite NTS054 Large 60.0% 35.7%
Inner
372 biotite NTS019 Large 70.0% 46.4%
Inner
374 biotite NTS019 Large 75.0% 52.6%
Outer
375 biotite NTS054 Small 78.0% 56.8%
210
Solid Solid
Outer
379 biotite NTS045 Small 70.0% 46.4%
Outer
380 biotite NTS045 Large 65.0% 40.8%
Outer
381 biotite NTS045 Large 60.0% 35.7%
Outer
382 biotite NTS045 Large 55.0% 31.2%
Outer
384 biotite NTS027 Large 75.0% 52.6%
Outer
385 biotite NTS027 Large 70.0% 46.4%
211
Solid Solid
212
Appendix B
Tables of rheology and sedimentation
data
A.1: Advanced argillic
Table B-1 shows the results for NTS037. SEQ numbers 158, 168 and 170 were used in subsequent
analysis. SEQ159 and SEQ160 were conducted on the s ame sample to investigate possible time effects.
As can be seen there was little to no variation in their rheology between t hese tests; each also
reported very little change in the area underneath their curves between the ramp up and ramp down
leading to the conclusion that advanced argillic is time independent. SEQ170 is presented here,
though, its rheological results are qual itative as the torque readings were all beneath the
manufacturers minimum torque reading or Taylor vortices were calculated. The val ue was therefore
calculated from the torque readings below the manufacturer’s recommendation. SEQ170 was not used
in any further rheology analysis because of the qualitative nature of the data; it is presented here
purely qualitatively.
213
Table B-1: NTS037 results
A.2: Argillic
Table B-2 shows the results for NTS038; all sequences were used in subsequent rheological
analysis. SEQ389 gave a relatively low R2 value, however, this could be converted into a p-value of
1.5E-06 v a l u e i n d i c a t i n g a v e r y h i g h p r o b a b i l i t y t h a t t h e f l o w c u r v e w a s r e a s o n a b l y a c c u r a t e .
214
Table B-2: NTS038 results
NTS049 is described by Table B-3; only SEQ215, SEQ216, and SEQ217 could be used for
subsequent rheological analysis. The apparent viscosity reported for SEQ218 and SEQ221 are both
qualitative, based off using the unrecommende d range of the rheometer. They are listed here for
demonstration purposes and are not used in any subse quent analysis. Using the Casson approximation
2 Overloaded, and the machine shopped early. As there was no down curve
215
on these low viscosity equations indicate that NTS049 becomes Newtonian by 31% solids
concentration
3 Very interesting curve. Time delay followed by a high speed slowing back down. Took sedimentation rate as being for the first hour
216
NTS108 as provided results are described in Table B-4 and its ground results Table B-5. As can
be seen the samples are slow settling and non -swelling. Although SEQ236 and SEQ251 indicate a low
R2, the associated p-values are 0.0012 and 5.2E-07 respectively indicating a reasonabl y close fit for
rheological purposes. They are subsequently used in later analysis. NTS108 after five minutes of
grinding has a 19% concentration which was used to evaluate the sedimentation rate.
5
SEQ233 is the same sample as SEQ232 except with an additional 4 minutes of mixing.
217
Table B-5: NTS108 Grind for 5 minutes
Table B-6 and Table B-7 contain NTS109 and NTS238 samples respectively. There was some
indication of swelling in NTS109 at 41% concentration; note, the mudline did not move yet 1 mL of
clear liquid formed on top of the mud layer. SEQ400 used the same sample as SEQ399; it was tested as
a side experiment to see how viscosity would change over several loop tests. The results are reported
in section 6.1 but is otherwise not used in any other test.
218
Table B-6: NTS109
1 mL of
396 41% 2.18 900 1.000 30.1 30 11% 0.0 liquid
6 Not used in regression analysis. It used the same sample as 399, it was a side experiment to see how the shear stress changed with additional loops.
219
Table B-7: NTS238
221
Table B-8: NTS008 results
196 41% 2.64 168 0.994 4.152 14.82 22% 1.5 Yes
Table B-9 and Table B-10 show the as provided and ground for five minutes results for NTS111.
The swelling information is complicated for the ground sample and is displayed in Table B-11. As can
8 All the data points were below the manual minimum torque; fitting the data to the Casson model
(despite the torque being out of range) found that the
substance was best described as Newtonian and that the entire region was beyond the maximum Taylor number
222
be seen grinding the samples significantly increases the swelling rate. SEQ182 and SEQ189 are
discussed in section 6.2; they use the same sample a s SEQ181 and are therefore not used in any other
subsequent rheology analysis. SEQ343, although it has a poor R2, its results have a low p -value
indicating suitability for further use. SEQ345, SEQ185, and SEQ187 are not used in any rheological
analysis. Unlike many of the other samples, NTS111 indicates time dependent shear thinning at high
concentrations whilst becoming shear thickening at lower concentrations. The a pparent shear
thickening behaviour coincides with the onset of sedimentation. As discussed elsewhere,
sedimentation can cause an apparent shear thickening behaviour as the bob can get caught on the
sediment.
223
Table B-9: NTS111 as provided results
1 mL
total
increase
in
341 53% 2 784 0.993 22.5 46 -15% 0.3 volume
342 46% 2.05 371 0.995 1.9 170 34% 5.0 None
9 p value=0.008
224
Table B-10: NTS111 after grinding for 5 minutes
225
Table B-11: Solids concentration and swelling details for NTS111 after grinding for 5 minutes
Solids Swelling
concentration
(v/v)
53% NA
Settled without the mud layer increasi ng. However, the total volume increased by
41% 1 mL
Settled without the mud level increasing. However, the total volume increased by
36% 1 mL
31% No swelling
Table B-12 shows the results for NTS239; the swelling is complicated, so it is described in more
detail in Table B-13. As is seen large levels of swelling can occ ur and swelling can clearly occur
during sedimentation.
226
Table B-12: NTS239 results
11 Not reliable
227
Table B-13: Solids concentration and swelling details for NTS239
Solids Swelling
concentration
(v/v)
53% NA
228
A.4: Silica Breccia
Table B-14 through Table B-17 show the results for the silica breccia samples (NTS010, NTS106
and NTS128). All were low viscosity slurries which were difficult to measure. SEQ354, SEQ340 and
SEQ267 are qualitative results and are not used for any rheological analysis because either all of their
torque readings were beneath the manu facturers minimum torque reading or Taylor vortices were
calculated.
229
Table B-14:NTS010 results
352 46% 2.03 322 0.999 6.5 43.53 29% 0.8 Yes
353 41% 2.11 108 0.982 2.4 11.99 37% 1.0 None
230
Table B-15: Solids concentration and swelling details for NTS010
Solids Swelling
concentration
(v/v)
41% None
36% None
231
Table B-16: NTS106 results
339 46% 2.71 379 0.996 4.0 111 46% 2.6 none
232
Table B-17: NTS128 results
8% None
233
A.5: Lower Epithermal
Lower Epithermal samples, seen in Table B-18 through Table B-23, were of relatively high
viscosities.
1 mL of
total
332 46% 2.91 1059 0.998 30.0 64 1% 0.2 volume
234
Table B-19: NTS110 results
235
Table B-20: Solids concentration and swelling details for NTS110
Solids Swelling
concentration
(v/v)
46% NA
Slurry settles by 2 mL but the total volume swells by 2 mL due to a liquid layer
31% forming on top
27% None
The sedimentation rates for SEQ298 and SEQ299 (see Table B-21) are for after the slurry had
finished swelling.
236
Table B-21: NTS110 after 5 minutes grinding
N A 12 46% NA NA NA NA NA NA NA NA
12 No rheology tests were performed as the suspension was too solid to feasibly load the rheometer
13 p value = 3.3E-5
237
Table B-22: Solids concentration and swelling details for NTS110 after five minutes of grinding
Solids Swelling
concentration
(v/v)
46% NA
41% NA
238
Table B-23: NTS240 results
288 46% 2.83 335 0.993 2.4 129 47% 5.1 None
239
A.6: Outer biotite
Outer biotite samples were quite variant as seen in Table B-24 to Table B-33. Of these samples:
• NTSO44 (after grinding for 5 minutes), NTS046, and NTS054 after grinding swelled.
• SEQ273, SEQ382, SEQ260, SEQ368, SEQ227, and SEQ228, SEQ321 and SEQ211 are not
used in any rheology analysis
240
Table B-24: NTS027 results
384 53% 7.3 451 0.995 5.9 108.11 27% 2.0 None
241
Table B-25: NTS044 ground for 5 minutes results
271 38% 6.01 240 0.996 8.1 7.48 11% 1.95 Yes
242
Table B-26: Solids concentration and swelling details for NTS044 after five minutes of grinding
Solids Swelling
concentration
(v/v)
46% NA
28% The mudline settled and the total volume increased by app roximately 4 mL
243
Table B-27: NTS045 results
380 41% 5.44 266 0.997 6.5 24.1 26% 2.1 None
14 p-value = 3.2x10-6.
244
Table B-28: NTS046 results
Yes
258 41% 3.86 317 0.999 9.0 19.36 19% 0.25 Yes
259 36% 4.05 111 0.980 3.5 4.43 -5% 2.5 Yes
16 Had to exclude a couple of outliers to generate the approximate viscosity. The shear stresses are outside of the rheometers range. The data is not used in
any rheology analysis
245
Table B-29: Solids concentration and swelling details for NTS046
Solids Swelling
concentration
(v/v)
53% NA
Slurry rises by 1 mL over 24 minutes and 30 seconds (2.4 mL / hour). The slurry
doesn’t settle but an additional 5 mL liquid layer forms on top of the mudline
46%
Liquid layer forms on top without the mud level increasing. The mudline
41% decreases after a very long time
31% None
Table B-30 contains the results for NTS054. As can be seen in the table, the SEQ numbers are
quite different at the same concentration. This is because the tests were performed on different dates
and from independently splitting the sample. Beneath 36% concentration (v/v) no useful flow curves
can be generated from the available data. At 41% the R 2 were relatively low, as such the p -values were
246
checked and found to be 5.4E-06 for SEQ226 and 5.4E-07 for SEQ367. As such, the data is viewed as
reliable.
247
Table B-30: NTS054 results
248
Table B-31: NTS054 after grinding for 5 minutes results
17 Not used as 324 was preferred as it was the older test. It is noteworthy the considerable differences in apparent viscosities.
18 Not reliable and thus not used in later analysis. Very complicated sedimentation
249
Table B-32: Solids concentration and swelling details for NTS054 after 5 minutes grinding
Solids Swelling
concentration
(v/v)
53% NA
Settled without mud layer increasing. However, the total volume increased by 4
46% mL
Settled without mud layer increasing. However, the total volume increased by 4
46% mL
Settled without mud layer increasing. However, the total volume increased by 2
42% mL
Settled without mud layer increasing. However, the total volume increased by 3
38% mL
Settled without mud layer increasing. However, the total volume increased by 1
31% mL
250
Table B-33: NTS100 results
19 Slows down rapidly after 13 minutes and 19 s. Took the sedimentation rate off those initial high speeds
251
A.7: Inner biotite
Table B-34 shows the results for NTS019; it was a fast settling slurry. The 46% concentrati on
was tested first and found to be fast settling. The high degree of time dependency is likely to be
because the sample settled around the bob during the test. Surprising, the sample was fluid underneath
the bob, and was relatively fluid above. An alterna tive ramping procedure was used for SEQ 374 were
the sample was ramped from 800 rpm to 10 without a loop test.
372 46% 6.15 77.465 1.000 0.5 33.47 32% 19.5 None
NTS055 is shown in Table B-35; like the other inner biotite samples NTS055 has low viscosity
and a high settling rate. Both SEQ279 and SEQ281 underwent sedimentation which began with a linear
252
profile before slowing down. S EQ279 began to slow after 16 minutes after having dropped 26 mL.
SEQ281 cannot be used for rheology analysis.
253
Table B-35: NTSS055 results
278 53% 6.42 515 0.992 3.4 211 25% 4.0 None
Table B-36, Table B-37, and Table B-38 show the results of NTS097 before and after grinding.
Only three SEQs need to be dismi ssed: SEQ241, SEQ243 and SEQ317. The as provided NTS097 did not
swell; after grinding for five minutes significant swelling occurred and is described in Table B-38.
21 Unreliable. Took the Newtonian viscosity; all data was clearly in the turbulent range.
254
Table B-36: NTS097 results
255
Table B-37: NTS097 after grinding for 5 minut es
22
No sedimentation was observed via the camera which recorded several hours of footage. However the slurry had settled over night by 3 mL
256
Table B-38: Solids concentration and swelling details for NTS097 after 5 minutes grinding
Solids Swelling
concentration
(v/v)
46% NA
42% M u d s e t t l e s b u t 3 m L o f l i q u i d f o r m s o n t o p 23
23 No sedimentation was observed via the camera. However the slurry had settled over night by 3 mL
257
Appendix C
Statistical results
A.8: Regression analysis of apparent viscosity vs
pH, concentration, passing 9.86, passing 38,
passing 53, amorphous silicate, kaolinite and clay
content
In the below regression analysis, the follo wing are used to
describe the variables:
Method
Rows 5
unused
258
Analysis of Variance
F- P-
Source DF Adj SS Adj MS Value Value
Regression 15 128.299 8.5532 22.35 0.000
Concentration 1 13.591 13.5909 35.51 0.000
Passing 9.86 1 11.625 11.6251 30.37 0.000
Passing 38 1 6.353 6.3535 16.60 0.000
Passing 53 1 3.230 3.2300 8.44 0.005
amorphous 1 0.115 0.1146 0.30 0.586
QXRD_Kaolinite 1 0.253 0.2535 0.66 0.418
Clay 1 0.009 0.0090 0.02 0.879
Concentration* 1 16.154 16.1543 42.21 0.000
Concentration
Passing 9.86*Passing 1 12.684 12.6840 33.14 0.000
9.86
amorphous*amorphous 1 2.307 2.3067 6.03 0.016
Concentration*Passing 1 6.540 6.5401 17.09 0.000
9.86
Concentration*Passing 1 3.288 3.2881 8.59 0.004
38
Concentration* 1 0.832 0.8324 2.17 0.144
QXRD_Kaolinite
Passing 9.86*Passing 1 11.142 11.1416 29.11 0.000
38
amorphous*Clay 1 3.121 3.1207 8.15 0.005
Error 83 31.768 0.3827
Total 98 160.067
Model Summary
R R- R-
S -sq sq(adj) sq(pred)
259
Coefficients
T- P-
Term Coef SE Coef Value Value VIF
Constant 19.05 4.53 4.20 0.000
Concentration -91.6 15.4 -5.96 0.000 366.74
Passing 9.86 -320.3 58.1 -5.51 0.000 4962.6
4
Passing 38 152.4 37.4 4.07 0.000 4820.2
1
Passing 53 22.80 7.85 2.90 0.005 232.29
amorphous -0.0135 0.0247 -0.55 0.586 40.50
QXRD_Kaolinite -0.118 0.146 -0.81 0.418 76.56
Clay 0.0049 0.0321 0.15 0.879 13.92
Concentration*Concentratio 94.5 14.5 6.50 0.000 235.24
n
Passing 9.86*Passing 9.86 874 152 5.76 0.000 7515.3
5
amorphous*amorphous 0.00121 0.00049 2.45 0.016 23.97
3 4
Concentration*Passing 9.86 407.4 98.6 4.13 0.000 1828.0
3
Concentration*Passing 38 -178.0 60.7 -2.93 0.004 1734.3
7
Concentration*QXRD_Kaolini 0.505 0.343 1.47 0.144 60.24
te
Passing 9.86*Passing 38 -548 102 -5.40 0.000 8380.2
8
amorphous*Clay - 0.00183 -2.86 0.005 11.78
0.00522
260
Regression Equation
η = 19.05 - 91.6 Concentration - 320.3 Passing 9.86 C-1
+ 152.4 Passing 38 + 22.80 Passing 53
- 0.0135 amorphous - 0.118 QXRD_Kaolinite
+ 0.0049 Clay
+ 94.5 Concentration*Concentration
+ 874 Passing 9.86*Passing 9.86
+ 0.001213 amorphous*amorphous
+ 407.4 Concentration*Passing 9.86
- 178.0 Concentration*Passing 38
+ 0.505 Concentration*QXRD_Kaolinite
- 548 Passing 9.86*Passing 38 -
0.00522 amorphous*Clay
R Large residual
X Unusual X
261
A.9: Regression analysis of the loga rithm of
apparent viscosity vs pH, concentration, passing
9.86, passing 38, passing 53, amorphous silicate,
kaolinite and clay content
• ln(𝜂)= l o g a r i t h m o f t h e a p p a r e n t v i s c o s i t y a t 5 0 m P a . s
Method
Rows 5
unused
262
Analysis of Variance
263
Model Summary
Coefficients
T- P-
Term Coef SE Coef Value Value VIF
Constant -13.25 1.27 -10.42 0.000
pH -0.405 0.246 -1.64 0.104 278.85
Concentration 15.71 1.44 10.94 0.000 21.63
Passing 9.86 -64.0 23.2 -2.76 0.007 5331.14
Passing 38 -154.1 32.3 -4.77 0.000 24305.1
9
Passing 53 197.0 31.8 6.20 0.000 25770.2
7
amorphous -0.0935 0.0143 -6.56 0.000 90.92
QXRD_Kaolinite -0.383 0.104 -3.70 0.000 262.70
Clay 0.0353 0.0154 2.28 0.025 21.85
pH*pH -0.0580 0.0184 -3.15 0.002 115.42
Passing 9.86*Passing -1631 343 -4.76 0.000 258911.
9.86 74
Passing 53*Passing 53 -692 117 -5.92 0.000 264604.
53
amorphous*amorphous 0.00208 0.00030 6.79 0.000 62.78
6 8
pH*Passing 9.86 -10.12 2.26 -4.47 0.000 1572.95
pH*Passing 38 8.19 1.45 5.67 0.000 1662.72
pH*amorphous 0.00421 0.00159 2.65 0.010 30.32
pH*QXRD_Kaolinite -0.0432 0.0158 -2.74 0.008 52.32
Concentration*Passing 10.96 3.53 3.10 0.003 43.94
53
264
T- P-
Term Coef SE Coef Value Value VIF
Passing 9.86*Passing 38 163 112 1.45 0.150 68599.1
8
Passing 9.86*Passing 53 1945 348 5.58 0.000 781356.
22
Passing 2.505 0.416 6.02 0.000 341.15
9.86*QXRD_Kaolinite
Regression Equation
ln(𝜂) = - 1 3 . 2 5 - 0 . 4 0 5 p H + 1 5 . 7 1 C o n c e n t r a t i o n - 6-1
64.0 Passing 9.86 - 154.1 Passing 38
+ 197.0 Passing 53 - 0.0935 amorphous -
0.383 QXRD_Kaolinite + 0.0353 Clay
- 0.0580 pH*pH -
1631 Passing 9.86*Passing 9.86 -
692 Passing 53*Passing 53
+ 0.002086 amorphous*amorphous -
10.12 pH*Passing 9.86 + 8.19 pH*Passing 38
+ 0.00421 pH*amorphous -
0.0432 pH*QXRD_Kaolinite
+ 10.96 Concentration*Passing 53
+ 163 Passing 9.86*Passing 38
+ 1945 Passing 9.86*Passing 53
+ 2.505 Passing 9.86*QXRD_Kaolinite
265
Fits and Diagnostics for Unusual Observations
R Large residual
266
Appendix D
Sizing data
The following pages contain tables recording the size
distribution data for each sample. Following these tables, there are
several figures which give the size distribution in graphical form.
267
268
269
270
Figure D-1:Advanced argillic cumulative passing si ze
271
Figure D-2: Argillic cumulative passing size
272
Figure D-4:Silica breccia cumulative passing size
273
Figure 5-5:Outer biotite cumulative passing size
274
Figure D-6:Inner biotite cumulative passing size
Appendix E
Data processing example
including raw data
An example of the data processing of SEQ233 is outlined here;
the raw data can be found in section A.13:. As stated earlier two
different data reduction procedures were used: the Estelle and Casson
approximation methods. Both methods contain some common early data
processing steps; the first of which is defining the measuring systems
characteristics and properties as in Table E-1 and Table E-2.
275
Table E-1: Measuring system characteristics of SEQ233. SEQ233
used the large bob and the RM180 rheometer in the wide gap
configuration described elsewhere in this thesis.
𝑘𝑔 Ρ 1871.7
Density ( )
𝑚3
Formula Value
Α 𝑟𝑐 1.666666667
=
𝑟𝑏
𝐾𝑏 = 2π. 𝑟12 . ℎ. 𝐹 8 . 0 3 6 9 1 E - 0 5
Table E-3 shows the averaging of the raw data and the shear
stress and angular speed calculations. Th e raw data is averaged at each
RPM from 10 data points as this helps smooth the results. If the RPM
was being held constant for longer than 10 s, then multiple aver aged
points are presented.
276
r γ̇ 1 τ f(τ)
Ω = ∫r 2 dr = − ∫τ 2 dτ 2-10
1 r 2 1 τ
Table E-3 Averaged raw data and the calculated shear stress and
angular velocity results.
277
RPM M (N.m) τ𝑏 ( P a ) τ𝑐 ( P a ) 𝑟𝑎𝑑𝑖𝑎𝑛𝑠
Ω ( )
(Averaged s
(Averaged
machine machine output)
output)
350 0.00523503 65.1 23.4 36.65
400 0.00544091 67.7 24.4 41.89
450 0.00563007 70.1 25.2 47.12
500 0.00582553 72.5 26.1 52.36
500 0.0059172 73.6 26.5 52.36
500 0.00599362 74.6 26.8 52.36
500 0.00604968 75.3 27.1 52.36
500 0.00614162 76.4 27.5 52.36
450 0.00602603 75.0 27.0 47.12
400 0.00588598 73.2 26.4 41.89
350 0.00572696 71.3 25.7 36.65
300 0.0055601 69.2 24.9 31.42
250 0.0053547 66.6 24.0 26.18
200 0.00511641 63.7 22.9 20.94
150 0.00483761 60.2 21.7 15.71
100 0.00447027 55.6 20.0 10.47
90 0.00440289 54.8 19.7 9.42
80 0.00433052 53.9 19.4 8.38
70 0.00425943 53.0 19.1 7.33
60 0.00414214 51.5 18.6 6.28
50 0.00401673 50.0 18.0 5.24
40 0.00388232 48.3 17.4 4.19
30 0.00371478 46.2 16.6 3.14
20 0.00351036 43.7 15.7 2.09
10 0.00318076 39.6 14.2 1.05
278
Table E-3 contains data points that need to be excluded; the
reduced data set is seen in Table E-4. There are two reasons why we
exclude data:
Table E-4: Data used for calculating shear rate. From Table E-3,
the last 5 rpm rate is treated as the equilibrium yield stress. At 500
rpm, the torque exceeded the manufacturers specification, so the data
point is omitted from further analysis.
𝑟𝑎𝑑𝑖𝑎𝑛𝑠
τ𝑏 ( P a ) Ω ( )
s
18.7 0.52
27.1 0.52
28.5 0.52
279
𝑟𝑎𝑑𝑖𝑎𝑛𝑠
τ𝑏 ( P a ) Ω ( )
s
29.1 0.52
29.7 0.52
30.2 0.52
33.2 1.05
37.8 2.09
40.4 3.14
42.4 4.19
43.9 5.24
45.3 6.28
46.4 7.33
47.9 8.38
48.9 9.42
49.9 10.47
53.6 15.71
56.9 20.94
59.9 26.18
62.5 31.42
65.1 36.65
67.7 41.89
70.1 47.12
72.5 52.36
73.6 52.36
74.6 52.36
280
𝑟𝑎𝑑𝑖𝑎𝑛𝑠
τ𝑏 ( P a ) Ω ( )
s
75.3 52.36
76.4 52.36
75.0 47.12
73.2 41.89
71.3 36.65
69.2 31.42
66.6 26.18
63.7 20.94
60.2 15.71
55.6 10.47
54.8 9.42
53.9 8.38
53.0 7.33
51.5 6.28
50.0 5.24
48.3 4.19
46.2 3.14
43.7 2.09
39.6 1.05
281
partially and fully sheared as seen respectively in the following two
equations:
𝑑Ω
𝛾̇ = 2𝑀 (𝑑𝑀) , 𝑖𝑓 τ2 < τ0 2-20
𝑑Ω 𝑑Ω
𝑀( ) Ω−𝑀( )
𝑑𝑀 𝑑𝑀
𝛾̇ = 2 𝑟2
− 𝑟1 , 𝑖𝑓 τ2 > τ0 2-21
1−( 12) ln( )
𝑟2
𝑟2
stress problem is avoided by the assumption that the true shear rate
occurs under the condition which maximises the energy dispensation,
i.e.
𝑑Ω 𝑑Ω
𝑑𝛺 𝑀( ) Ω−𝑀( )
𝑑𝑀 𝑑𝑀
𝛾̇ = max (2 𝛺 ;2 𝑟 2 − 𝑟b ) E-1
𝑑𝑀 ln( )
1−( b ) 𝑟𝑐
𝑟2c
Figure 4-3; the R2 value is almost 1 yet as can be seen in Table E-5
there was a negative derivati ve of angular speed against torque. As
described in section 4.9.2 taking higher order fits could overcome
these problems but at the expense of possibly overfitting the data.
282
Figure 4-3: Angular speed vs torque for SEQ233.
283
Table E-5 : The components required for the Estelle
approximation. Highlighted in red is the physically impossible result
𝑑𝛺
of a negative .
𝑑𝑀
𝑟𝑎𝑑𝑖𝑎𝑛𝑠 𝑑Ω
τ𝑏 ( P a ) Ω ( ) = 10𝐸 +07 𝑀 − 25072
s 𝑑𝑀
284
This could be avoided by splitting the curve into multiple
components. Table E-6 shows how SEQ233 was split into three parts:
𝛺 = 𝑎2 𝜏 2 + 𝑎1 𝜏 + 𝑎0 E-2
285
Table E-7: The shear rate calculation using the Estelle method.
𝛾̇
𝑟𝑎𝑑𝑖𝑎𝑛𝑠 𝑑Ω
τ𝑏 ( P a ) Ω ( )
s Part of the curve 𝑑𝑀 Partial Fully Max
286
56.9 20.94 21065 192.8 153.5 192.8
287
The final steps are calculating the apparent viscosity and
trimming the data to exclude shear rates which have a Taylor number
above 41.3.
𝜏
𝜂𝑎𝑝𝑝𝑎𝑟𝑒𝑛𝑡 = 𝛾̇ 2-1
41.3 < 𝑇𝑎 < 400 ∶ 𝑙𝑎𝑚𝑖𝑛𝑎𝑟 𝑓𝑙𝑜𝑤 𝑤𝑖𝑡ℎ 𝑇𝑎𝑦𝑙𝑜𝑟 𝑣𝑜𝑟𝑡𝑖𝑐𝑒𝑠 3-4
w h e r e U𝑏 = Ω. 𝑟𝑏
288
Table E-8: Calculating the Taylor number with the Estelle method. The red lines indicate cells
with Taylor vortices
289
τ𝑏 ( P a ) 𝑟𝑎𝑑𝑖𝑎𝑛𝑠 𝛾̇ 𝜂𝑎𝑝𝑝𝑎𝑟𝑒𝑛𝑡 Ub Taylor fully sheared
Ω ( )
s
290
The final results of the Estelle approximation are presented
in Table E-9. The shear rates for the original yield stress test and
the hysteresis loop are included and were assumed to be equal to
the shear rates at the equivalent rpm. This allows the exploration
of any time dependency.
291
Table E-9: Final result from the Estelle calculation
τ𝑏 ( P a ) 𝑟𝑎𝑑𝑖𝑎𝑛𝑠 𝛾̇ 𝜂𝑎𝑝𝑝𝑎𝑟𝑒𝑛𝑡
RPM M Ω ( )
s
292
τ𝑏 ( P a ) 𝑟𝑎𝑑𝑖𝑎𝑛𝑠 𝛾̇ 𝜂𝑎𝑝𝑝𝑎𝑟𝑒𝑛𝑡
Ω ( )
RPM M s
293
To compare the relative viscosities of different samples, a shear
rate of 50 s-1 was selected. The exact selection of 50 s -1 was due to a
combination of
1 1 1
Ω = 2η ( (1 − α2)τ1 − 4(1 − α)√τ0 τ1 + 2τ0 ln(α)) 4-4
∞
1. Set the yield stress and the infinite viscosity of the fluid
294
2. Calculate whether, at a given shear stress, th e fluid is fully
or partially yielded. This is done by calculating the r adial
distance (d) that the fluid would be sheared if the bob was
placed in an infinite medium.
τ1
𝑑 = 𝑟1 . √
τ0
a . 𝜂∞ > 0.001; a s t h e v i s c o s i t y o f a s u s p e n s i o n c a n n o t b e
smaller than the carrying fluid.
b . 𝜏𝑦 ≥ 0; a s n e g a t i v e y i e l d s t r e s s i s p h y s i c a l l y i m p o s s i b l e .
295
6. Calculate the R2 value using Excel’s CORREL fu nction. The
CORREL function only calculates R, so it will need to be
squared.
I n f i n i t e v i s c o s i t y ( 𝜂∞ ; 𝑃𝑎. 𝑠) 0.0304
Y i e l d s t r e s s ( 𝜏𝑦 ; 𝑃𝑎) 26.88
296
τ𝑏 ( P a ) Yielding 𝑟𝑎𝑑𝑖𝑎𝑛𝑠 (𝛺𝑀𝑒𝑎𝑠𝑢𝑟𝑒𝑑,𝑖
𝛺( )
distance s − 𝛺𝑃𝑟𝑒𝑑𝑖𝑐𝑡𝑒𝑑,𝑖 )2
1 2
𝛾̇ = 𝜂 . (√τ1 − √τ0 ) E-3
∞
𝑑∗Ub ∗ρ d
Ta = ∗ √𝑟 E-4
η b
w h e r e U𝑏 = Ω. 𝑟𝑏
297
Table E-12: The Taylor number calculation technique. Note, for this example, the shearing is
always partial due to the high y ield stress. Under the fully sheared condition the distance would be
0.01 m
τ𝑏 (Pa) Ub 1 η d=Shearing distance (m) Taylor number
𝛾̇ ( )
s
30.2 0.008 3.3 9.29 0.0009 0.0
33.2 0.016 11.0 3.02 0.0017 0.0
37.8 0.031 30.3 1.25 0.0028 0.0
40.4 0.047 44.9 0.90 0.0034 0.1
42.4 0.063 57.9 0.73 0.0038 0.3
43.9 0.079 68.4 0.64 0.0042 0.4
45.3 0.094 78.6 0.58 0.0045 0.7
46.4 0.110 87.2 0.53 0.0047 0.9
47.9 0.126 99.6 0.48 0.0050 1.2
48.9 0.141 107.6 0.45 0.0052 1.6
49.9 0.157 116.1 0.43 0.0054 2.0
53.6 0.236 150.6 0.36 0.0062 4.3
56.9 0.314 183.4 0.31 0.0068 7.7
59.9 0.393 214.8 0.28 0.0074 12.0
62.5 0.471 243.3 0.26 0.0079 17.2
65.1 0.550 274.2 0.24 0.0083 23.7
67.7 0.628 304.9 0.22 0.0088 31.3
70.1 0.707 334.0 0.21 0.0092 39.9
72.5 0.785 364.8 0.20 0.0096 50.1
298
Since there were possible vortices, the procedure was
iterated. The results are shown in Table E-13, Table E-13 and
Table E-14.
I n f i n i t e v i s c o s i t y ( 𝜂∞ ; 𝑃𝑎. 𝑠) 0.0295
Y i e l d s t r e s s ( 𝜏𝑦 ; 𝑃𝑎) 27.10
299
Table E-15: Taylor data
τ𝑏 (Pa) Ub 1 η Shearing distance (d) Taylor number
𝛾̇ ( )
s
30.2 0.008 2.9 10.36 0.0008 0.0
33.2 0.016 10.5 3.15 0.0016 0.0
37.8 0.031 29.8 1.27 0.0027 0.0
40.4 0.047 44.6 0.91 0.0033 0.1
42.4 0.063 57.8 0.73 0.0038 0.3
43.9 0.079 68.3 0.64 0.0041 0.4
45.3 0.094 78.7 0.58 0.0044 0.6
46.4 0.110 87.5 0.53 0.0046 0.9
47.9 0.126 100.0 0.48 0.0050 1.2
48.9 0.141 108.2 0.45 0.0051 1.5
49.9 0.157 116.8 0.43 0.0054 1.9
53.6 0.236 152.0 0.35 0.0061 4.3
56.9 0.314 185.4 0.31 0.0067 7.6
59.9 0.393 217.4 0.28 0.0073 11.9
62.5 0.471 246.5 0.25 0.0078 17.1
65.1 0.550 278.0 0.23 0.0083 23.6
67.7 0.628 309.4 0.22 0.0087 31.3
70.1 0.707 339.1 0.21 0.0091 39.9
300
As can be seen in Table E-15 no other shear stresses contain
Taylor numbers above 41.3.
The final step was step 6, where the R2 value was found using
Excel’s inbuilt CORREL function. A plot of the graph can be seen in
Figure E-1.
A.12: Summary
The data processing procedure was outlined using SEQ233 as an
example. A comparison between the different calculation techniques is
provided in Figure E-2; as can be seen both the Estelle and Casson
methods produce similar answers. The Newtonian approximation is
also included; its equation is given by:
302
2Ω. 𝑟𝑐2
𝛾̇ =
𝑟𝑐2 − 𝑟𝑏2
• its automatable;
• consistent;
• verifiable;
303
A.13: Raw data for SEQ233
Raw results for SEQ233
5 0.00018773 21.044
5 0.00073941 21.036
5 0.0012379 21.036
5 0.0014994 21.036
5 0.0016697 21.021
5 0.0017566 21.044
5 0.001924 21.021
5 0.0019663 21.044
5 0.0020058 21.029
5 0.002041 21.014
5 0.0021316 21.021
5 0.0021201 21.029
5 0.0021344 21.029
5 0.0020899 21.014
5 0.0021366 20.991
5 0.0022314 20.999
5 0.0021998 21.021
5 0.0022221 20.999
5 0.0022817 21.014
5 0.0022494 21.029
5 0.002268 21.006
5 0.0022041 21.006
304
Raw results for SEQ233
5 0.0022156 20.999
5 0.0023262 21.029
5 0.0023176 21.014
5 0.0022343 21.014
5 0.0022889 20.999
5 0.0023291 20.999
5 0.0023262 21.014
5 0.0023751 20.969
5 0.0023176 20.984
5 0.0022946 20.984
5 0.0023025 20.999
5 0.0022846 20.976
5 0.0022882 20.991
5 0.002462 20.984
5 0.002406 20.999
5 0.0023765 20.969
5 0.0023399 20.961
5 0.0023255 20.954
5 0.0023787 20.991
5 0.0024246 20.969
5 0.0023621 20.961
5 0.0023277 20.976
5 0.0023736 20.976
305
Raw results for SEQ233
5 0.0024096 20.947
5 0.0024081 20.969
5 0.0024139 20.961
5 0.0023751 20.969
5 0.0024139 20.976
5 0.0024879 20.947
5 0.0025202 20.954
5 0.0023801 20.954
5 0.0023851 20.932
5 0.0024699 20.961
5 0.0024354 20.969
5 0.0023765 20.939
5 0.002406 20.961
5 0.0023952 20.947
5 0.0024498 20.961
10 0.0025863 20.917
10 0.0026006 20.947
10 0.0026552 20.947
10 0.0026725 20.917
10 0.0026006 20.947
10 0.0026983 20.887
10 0.0026955 20.917
10 0.002661 20.917
306
Raw results for SEQ233
10 0.0027673 20.917
10 0.0027587 20.947
20 0.0029791 20.917
20 0.0029532 20.947
20 0.0030653 20.887
20 0.0030021 20.887
20 0.0030365 20.887
20 0.0030538 20.917
20 0.003071 20.917
20 0.003071 20.947
20 0.0030624 20.917
20 0.0030452 20.917
30 0.0032441 20.887
30 0.0032326 20.887
30 0.0032613 20.917
30 0.0032527 20.917
30 0.003224 20.887
30 0.0032613 20.917
30 0.0032182 20.976
30 0.0032786 20.917
30 0.0032125 20.917
30 0.0032499 20.887
40 0.0034255 20.917
307
Raw results for SEQ233
40 0.0033737 20.887
40 0.0033623 20.917
40 0.0034341 20.887
40 0.0033766 20.917
40 0.0034513 20.857
40 0.0033737 20.857
40 0.0034255 20.887
40 0.003437 20.857
40 0.0034168 20.917
50 0.0035481 20.887
50 0.0035193 20.917
50 0.0035107 20.917
50 0.0035193 20.917
50 0.0034992 20.887
50 0.0035481 20.917
50 0.003528 20.887
50 0.0035538 20.887
50 0.0035136 20.827
50 0.0035452 20.857
60 0.0036356 20.857
60 0.0036212 20.857
60 0.0036298 20.887
60 0.0036356 20.887
308
Raw results for SEQ233
60 0.0036586 20.857
60 0.00367 20.857
60 0.0036499 20.857
60 0.0036183 20.887
60 0.0036212 20.857
60 0.0036643 20.917
70 0.0035733 20.827
70 0.0037773 20.887
70 0.0037227 20.887
70 0.0037313 20.887
70 0.0037543 20.857
70 0.0037256 20.857
70 0.0037801 20.857
70 0.0037457 20.857
70 0.0037342 20.827
70 0.0037572 20.857
80 0.0038785 20.857
80 0.0038239 20.857
80 0.0038757 20.827
80 0.0038785 20.857
80 0.0038699 20.857
80 0.0038757 20.827
80 0.0038354 20.827
309
Raw results for SEQ233
80 0.0038412 20.827
80 0.0038239 20.857
80 0.0038297 20.827
90 0.0039308 20.857
90 0.0039423 20.857
90 0.0039222 20.827
90 0.0039394 20.827
90 0.0039365 20.827
90 0.0039193 20.827
90 0.0039365 20.857
90 0.0039279 20.857
90 0.0039078 20.857
90 0.0039365 20.827
310
Raw results for SEQ233
311
Raw results for SEQ233
312
Raw results for SEQ233
313
Raw results for SEQ233
314
Raw results for SEQ233
315
Raw results for SEQ233
316
Raw results for SEQ233
317
Raw results for SEQ233
318
Raw results for SEQ233
90 0.0043963 20.797
90 0.004402 20.797
90 0.0043762 20.797
90 0.0043963 20.797
90 0.0043934 20.797
90 0.004402 20.797
90 0.0043991 20.767
319
Raw results for SEQ233
90 0.0044078 20.767
90 0.004448 20.797
90 0.0044078 20.797
80 0.0043182 20.797
80 0.0043153 20.767
80 0.00439 20.797
80 0.0043239 20.797
80 0.0043411 20.797
80 0.0043153 20.797
80 0.0043124 20.767
80 0.0043498 20.797
80 0.0043268 20.797
80 0.0043124 20.797
70 0.0042054 20.767
70 0.0042284 20.797
70 0.0042456 20.767
70 0.0043002 20.767
70 0.0042514 20.797
70 0.0042974 20.767
70 0.0042571 20.737
70 0.004306 20.797
70 0.0042744 20.827
70 0.0042284 20.767
320
Raw results for SEQ233
60 0.0041298 20.767
60 0.0041585 20.797
60 0.0041413 20.737
60 0.0041413 20.767
60 0.0041269 20.767
60 0.0041355 20.797
60 0.0041499 20.767
60 0.0041413 20.767
60 0.0041154 20.767
60 0.0041815 20.797
50 0.003982 20.737
50 0.0039992 20.767
50 0.0040337 20.767
50 0.0040107 20.797
50 0.0040279 20.797
50 0.0039992 20.737
50 0.0040193 20.767
50 0.0040251 20.767
50 0.0040423 20.797
50 0.0040279 20.797
40 0.0039139 20.737
40 0.0038593 20.797
40 0.0038306 20.767
321
Raw results for SEQ233
40 0.0039111 20.737
40 0.003845 20.737
40 0.0038737 20.797
40 0.0038507 20.797
40 0.0039513 20.767
40 0.0039053 20.797
40 0.0038823 20.737
30 0.0037326 20.767
30 0.0037584 20.767
30 0.0036924 20.767
30 0.003724 20.767
30 0.0036694 20.737
30 0.0037125 20.797
30 0.0036751 20.767
30 0.0037671 20.737
30 0.003701 20.767
30 0.0037153 20.797
20 0.0034618 20.737
20 0.0034963 20.797
20 0.0035595 20.708
20 0.0035279 20.767
20 0.0035336 20.767
20 0.0034589 20.767
322
Raw results for SEQ233
20 0.0035221 20.797
20 0.0035279 20.797
20 0.0035308 20.737
20 0.0034848 20.797
10 0.0031839 20.797
10 0.0031351 20.767
10 0.003204 20.797
10 0.0031696 20.737
10 0.0032155 20.737
10 0.0031954 20.737
10 0.0031552 20.737
10 0.0031839 20.737
10 0.0032127 20.767
10 0.0031523 20.767
Appendix F
Sedimentation curves
Please see attached document labelled
s4464068_MPhil_thesis_supplementary1.pdf
323
Appendix G
Flow curves
Please see attached document labelled
s4464068_MPhil_thesis_supplementary2.pdf
324