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Use of the Scanning Electron Microscope to

Determine the Sampling Constant and


Liberation Factor for Fine Minerals
Geoffrey J Lyman
Materials Sampling & Consulting Pty Ltd, Australia
Robert Schouwstra
Anglo Research, Johannesburg, South Africa
In memory of Pedro Carrasco Castelli
Motivation
• For the design of sampling and analysis protocols for
fine mineral samples it is necessary to have a
sampling constant for the solids with respect to all
analytes of interest

2 2
KS 3
  x  c l fg d 9 5
MS

• But knowing the sampling constant, the size


distribution, the mode of occurrence of the minerals
and the head assay, the liberation factor for a size
fraction can be calculated
Motivation
• The traditional means of finding the sampling constant at a
given state of comminution is to carry out replicate analyses
of samples at various mass levels and then examine the
dependence of sampling variance on sample mass
– this technique is time consuming
– corrections for the analytical variance must be made

• The sampling constant may also be estimated from the shape


factor, f, size factor, g, mineralogical composition factor c,
material top size, d3 and the liberation factor l
• The difficulty is in finding the correct value of l.
Motivation
• The automated scanning electron microscope (SEM)
(QEMSCAN or MLA) can be used to collect highly detailed
information from particle sections
Method
• The fundamental information from the SEM is the area of
each mineral type (or group of minerals) contained in each
particle
• If the areal fraction in the particle is equated to volume
fraction and the phase densities are known, a mass
composition of each particle can be calculated with respect to
phases or, with the mineral elemental analysis, elements
• This is the information needed to find the sampling constant
for the sample under scrutiny with respect to all defined
phases or elements of interest
Method
• The sampling constant is given, fundamentally, by
N pi 2
Ns  a ij 
KS   xivi  y ij  ij 
 a
 1

i1 j1  S 
th
x i  m a s s fr a c tio n o f p a r tic le s in i s iz e fr a c tio n
th
v i  v o lu m e o f ty p ic a l p a r tic le in i s iz e fr a c tio n
th th
y ij  m a s s fr a c tio n o f j p a r tic le in i s iz e fr a c tio n
th th
 ij  d e n s ity o f j p a r tic le in i s iz e fr a c tio n
th th
a ij  a s s a y o f j p a r tic le in i s iz e fr a c tio n w .r .t. p h a s e o r e le m e n t o f in te r e s t

a S  s a m p le a s s a y w .r .t. p h a s e o r e le m e n t o f in te r e s t
N p i  n u m b e r o f p a r t ic le s in s iz e fr a c tio n in te r r o g a te d

N s  n u m b e r o f s iz e fr a c tio n s d e fin e d
Method
• The liberation factor for a mineral phase in a size fraction can
be found by comparing the heterogeneity of a size fraction
with the heterogeneity of that fraction if the phase(s) of
interest were fully liberated
• The heterogeneity of a size fraction can be written as
N pi 2
 a ijk 
IH k i   y ij  ij 
 a
 1

j1  k 
and with full liberation of the phase
  a k  m e a n m a s s fra c tio n o f
 1 
IH ik m a x   1  ak    k   1    ik o 
 p h a s e k in s a m p le
  ak  
 ik o  m e a n d e n s ity o f a ll o th e r

p h a s e s in th e fra c tio n
Method
• The liberation factor for the kth phase in the ith size fraction is
then
IH ik
l ik

IH ik m ax

• Note that we do not need this number to calculate the


sampling constant, but it is of interest to know what it is
• It may also have value to the metallurgists when calculated for
a concentrate or tailings sample
Results
• Sampling Constants for Phases
Particle Intrinsic Heterogeneity [gm cm-3]
Size fraction
% [w/w] Volume
[microns] Min_a Min_b Min_c Min_d Min_e Min_f Min_g Min_h
[cm3]
2360 1180 20.73 3.70E-03 0.270 0.652 9.739 2.883 5.6 28.1 4.3 5.7
1180 850 22.05 5.64E-04 0.521 1.097 33.509 11.962 4288.4 124.0 420.3 11.2
850 600 9.92 2.08E-04 0.901 1.584 54.355 17.463 1400.3 63.6 1028.4 192
600 425 8.16 7.32E-05 1.066 1.796 50.239 20.155 1258.1 150.0 152.3 1109
425 212 20.29 2.16E-05 2.065 3.451 83.143 24.017 1431.3 150.7 2799.9 53502
212 106 11.53 2.68E-06 2.677 4.599 60.130 21.226 1041.2 79.7 664.6 191652
106 10 7.32 2.98E-07 3.493 5.594 96.406 17.679 1113.4 121.6 439.4 1013490
Ks [gm] 3.06E-04 6.96E-04 1.34E-02 4.29E-03 5.81E-01 3.98E-02 9.01E-02 3.32E-01

• For Elements Size fraction


[microns]
% [w/w]
Particle
Volume
[cm3] El_a
Intrinsic Heterogeneity [gm cm-3]
El_b El_c El_d
2360 1180 20.73 3.70E-03 0.305 0.127 0.539 0.026
1180 850 22.05 5.64E-04 0.472 0.550 0.930 0.094
850 600 9.92 2.08E-04 0.681 1.020 1.406 0.124
600 425 8.16 7.32E-05 0.762 1.216 1.542 0.138
425 212 20.29 2.16E-05 1.482 2.076 3.080 0.182
212 106 11.53 2.68E-06 1.953 2.357 3.971 0.137
106 10 7.32 2.98E-07 2.322 3.271 4.876 0.121
Ks [gm] 3.18E-04 2.04E-04 5.82E-04 3.58E-05
Results
• Liberation Constants for Phases, by size

Size fraction Liberation Factor


% [w/w]
[microns] Min_a Min_b Min_c Min_d Min_e Min_f Min_g Min_h
2360 1180 20.73 0.050 0.076 0.016 0.027 0.003 0.037 0.001 0.000
1180 850 22.05 0.096 0.129 0.054 0.110 2.143 0.162 0.141 0.000
850 600 9.92 0.166 0.186 0.088 0.161 0.700 0.083 0.345 0.0006
600 425 8.16 0.196 0.211 0.082 0.186 0.629 0.196 0.051 0.0038
425 212 20.29 0.382 0.406 0.135 0.221 0.715 0.197 0.940 0.185
212 106 11.53 0.499 0.543 0.098 0.195 0.520 0.104 0.223 0.663
106 10 7.32 0.654 0.663 0.156 0.163 0.556 0.159 0.148 3.506
Results
• Liberation Constants for Phases, by size

Size fraction Liberation Factor


% [w/w]
[microns] Min_a Min_b Min_c Min_d Min_e Min_f Min_g Min_h
2360 1180 20.73 0.050 0.076 0.016 0.027 0.003 0.037 0.001 0.000
1180 850 22.05 0.096 0.129 0.054 0.110 2.143 0.162 0.141 0.000
850 600 9.92 0.166 0.186 0.088 0.161 0.700 0.083 0.345 0.0006
600 425 8.16 0.196 0.211 0.082 0.186 0.629 0.196 0.051 0.0038
425 212 20.29 0.382 0.406 0.135 0.221 0.715 0.197 0.940 0.185
212 106 11.53 0.499 0.543 0.098 0.195 0.520 0.104 0.223 0.663
106 10 7.32 0.654 0.663 0.156 0.163 0.556 0.159 0.148 3.506
Results
• Liberation Constants for Phases, by size (major phases)
Results
• Liberation Constants for Phases, by size (minor phases)
Results
• Particle Density Distributions
Particle Distribution for Particle Distribution for Particle Distribution for Particle Distribution for
2360x1180micron 1180x850micron 850x600micron 600x425micron
25 250 600 800

20 200 500
600
400
15 150
Count

Count

Count

Count
300 400
10 100
200
200
5 50 100
0 0 0 0
Density Density Density Density

Particle Distribution for Particle Distribution for Particle Distribution for 106x10micron
425x212micron 212x106micron
5000
2500 3000
4000
2000 2500
2000 3000

Count
1500
Count

Count

1500
1000 2000
1000
500 1000
500
0 0 0
Density Density Density
Results
• Particle Composition Distributions (Mineral a)
Min_a 2360x1180micron Min_a 1180x850micron Min_a 850x600micron Min_a 600x425micron
0.12 0.07 0.06 0.05

Mass Fraction of Particles

Mass Fraction of Particles


Mass Fraction of Particles

Mass Fraction of Particles


0.10 0.06 0.05 0.04
0.08 0.05 0.04
0.04 0.03
0.06 0.03
0.03 0.02
0.04 0.02 0.02
0.02 0.01 0.01
0.01
0.00 0.00 0.00 0.00
0 0.5 1 0 0.5 1 0 0.5 1 0 0.5 1

Mass Fraction of Phase Mass Fraction of Phase Mass Fraction of Phase Mass Fraction of Phase

Min_a 425x212micron Min_a 212x106micron Min_a 106x10micron


0.04 0.08 0.20
Mass Fraction of Particles
Mass Fraction of Particles

Mass Fraction of Particles


0.03 0.06 0.15

0.02 0.04 0.10

0.01 0.02 0.05

0.00 0.00 0.00


0 0.5 1 0 0.5 1 0 0.5 1

Mass Fraction of Phase Mass Fraction of Phase Mass Fraction of Phase


Conclusions
• Automated SEMs can collect data that can be used directly for
sampling calculations
• The sampling constant is calculated directly for phases or
elements with no correction for analytical variance
• Rare phases present some difficulty, but the SEMS can do rare
component searches – or a proxy phase can be used
• Particles up to 5 mm in size can be analysed

Many thanks to friends and colleagues


at Anglo Research for permission to
publish