121

Canadian Metallurgical Quarterly, Vol 39, No 2, pp 121-128, 2000

© Canadian Institute of Mining, Metallurgy and Petroleum
Published by Canadian Institute of Mining, Metallurgy and Petroleum
Printed in Canada. All rights reserved

A STANDARD MATERIAL FOR STEREOLOGICAL CORRECTION

D. LIN1 and J.A. FINCH2
1
Cominco Ltd., P.O. Box 2000, Trail, B.C., Canada, V1R 4S4
2
McGill University, Department of Metallurgical Engineering, 3610 University St. Montreal, Quebec,
Canada, H3A 2B2

(Received March 1999; in revised form September 1999)

Abstract — The determination of mineral liberation by microscopic examination of ore particle sections
is stereologically biased. Procedures have been developed to correct this bias, but most have not been
thoroughly tested. A standard material, a material of known particle composition and locking character-
istics, would allow the proper testing of these procedures. In this work, a method was developed for the
creation of a standard material consisting of two phases: glass and lead borate. Simple-locked particles
and particles with granular and layered textures can be created. The standard material is versatile and
easy to use.

Résumé — La détermination de la libération de minéraux par examen microscopique de sections de

particule de minerai est biaisée stéréologiquement. Des procédures on été développées afin de corriger
ce biais, mais la plupart n'ont pas été entièrement évaluées. Un matériel étalon, un matériel de
composition de particules et de caractéristiques d'emprisonnement connues, permettrait une évaluation
appropriée de ces procédures. Dans ce travail, on a développé une méthode pour la création d'un matériel
étalon consistant de deux phases: verre et borate de plomb. Des particules à emprisonnement simple et
des particules avec des textures granulaires et avec couches peuvent être créées. Le matériel étalon est
versatile et facile à utiliser.

INTRODUCTION For the standard material, a two-phase (binary) system

Mineral liberation represents the ultimate limit in the separa-
bility of mineral phases. The measurement of mineral libera-
tion is usually accomplished by mounting the particles in a
resin matrix, polishing a surface and examining the surface
with an optical or electron microscope. Images of the surface
are digitised and processed with an image analyser. The image
analyser measures the liberation by determining the mineral
composition of the individual particle sections. This method of
measuring liberation is stereologically biased. Liberated parti-
cles will always yield liberated sections whereas locked parti-
cles can yield liberated or locked sections. As a result, miner-
al liberation will always be over-estimated.
is all that is required because liberation is measured one
phase at a time: while the liberation of one mineral phase is
being measured, the rest of the mineral phases in the sam-
ple can simply be grouped together as the second phase. A
true, two-phase material is essential if density fractionation
of the particles is performed to provide the independent and
true measure of particle composition. If there are more than
two phases, there will not be a direct correlation between
particle density and particle composition. Obviously, a sig-
nificant density difference between the two phases is nec-
essary to provide good resolution to the density splits. A
near-perfect separation such as that obtained using heavy
liquids is desired to ensure the precision of the splits.

Methods have been developed to correct the stereological
bias [1, 2, 3, 4, 5, 6, 7], but the effectiveness of these methods
is difficult to test since the true liberation is not known.
Standard materials, that is, materials of known particle libera-
tion and locking characteristics, have been developed in an
attempt to allow the assessment of these correction proce-
dures. The present work describes a method of producing a
versatile standard material that can be used to test the robust-
ness of stereological correction procedures.
For the standard material, there must be a method of
distinguishing the two phases. If optical microscopy is
used, the two phases must be different colours or have
some other differentiating feature. If electron microscopy is
used, the two phases must have different grey levels when
viewed with backscattered electron imaging. The backscat-
tered grey level of a phase is directly related to its average
atomic number such that a low atomic number material will
appear dark and a high atomic number material will appear
CANADIAN METALLURGICAL QUARTERLY
122 D. LIN and J.A. FINCH
bright. In this work, the standard material was designed for
use with electron microscopy.
It is desirable that the standard material be able to
exhibit simple locking (i.e., only one interface between the
phases in the particle). Simple locking is probably the most
important of all locking types in mineral processing fol-
lowing the argument that since comminution is aimed at
creating free particles, the mineral which fails to be liberat-
ed is most likely concentrated in the next simplest class -
the simple-locked particle class. Simple locking also cre-
ates the most severe stereological bias and is, therefore, a
severe test of any stereological correction procedure [1,2].
The standard material should also be flexible enough to
simulate different types of locking textures. Although a
stereological correction procedure may be effective with
one type of locking texture, it may not be as effective with
others. In addition, it would be instructive to examine the
effect of locking texture on the predictive abilities of dif-
ferent liberation models.
There are two categories of standard materials: natural-
ly-occurring and artificial. A short review of previous
attempts to create standard materials follows.
STANDARD MATERIAL PREPARATION
A SHORT REVIEW
Naturally-occurring standard materials
Naturally-occurring standard materials are created from
naturally-occurring two-phase ores. The ore is broken,
screened and the composition of the particles measured by
density fractionation. There have been several efforts to
develop a standard material from natural sources, but there
are difficulties in finding a two-phase ore whose phases are
free from porosity and impurities. If there are significant
quantities of either of these in the particles then the deter-
mination of particle composition from density measure-
ments is not accurate. Similarly, this would be a problem if
there were variations in the density of either of the two
phases. The use of a naturally-occurring standard material
is limited because the locking texture cannot be controlled.
Work performed in this area is described below.
1. Stewart and Jones [8] used a siliceous iron ore which
consisted of grains of iron oxides (hematite with magnetite
and minor amounts of goethite and limonite) in a siliceous
matrix (quartz with minor amounts of other silicates). The
ore was crushed to 90% -1.0 mm and screened. The parti-
cles were separated based on density using heavy liquids
(for densities below 3.32 g/ml) and a fluidised bed (for den-
sities above 3.32 g/ml). The siliceous material was estimat-
ed to have a density of 2.65 g/ml and the iron oxides to
have a density of 5.06 g/ml. There were two problems with
this standard material: there may have been significant
CANADIAN METALLURGICAL QUARTERLY
porosity in the ore [6(p.118)] and there was some variation
in the density of the iron minerals.
2. Bole et al. [9] examined two binary ores: an iron-
oxide/silicate sample and a sphalerite/dolomite sample.
Both ores were crushed and screened to 417-595 µm and
the iron-oxide/silicate particles fractionated using heavy
liquids. The densities of the silicate and iron oxide phases
were 2.72 and 5.10 g/ml, respectively. The sphalerite/dolomite
particles were density fractionated using the Magstream
separator (a centrifugal magnetogravimetric separator).
The density of the dolomite was 2.85 g/ml and that of the
sphalerite, 4.00 g/ml.
3. Miller and Lin [10] used a unique approach to deter-
mining the true liberation of mineral particles. They used
serial sectioning to determine the liberation of an iron ore
and a copper ore. Particles were screened to 74-105 µm and
mounted in resin. By polishing this pellet down by intervals
of 18 µm, a series of parallel sections was gathered for each
particle. The composition of each particle was reconstruct-
ed based on these sections. Although serial sectioning does
provide an unbiased measure of the true liberation distrib-
ution, it is too tedious and expensive to use in regular lib-
eration analyses.
Artificial standard materials
The general procedure to create an artificial standard mate-
rial is summarised in Figure 1. Monosize grains of one
phase are embedded into a matrix which acts as the second
phase. The matrix phase is usually a plastic or resin in liq-
uid form. When the plastic hardens, a two-phase block is
formed. The block is then crushed producing free and
locked particles. These particles are screened into different
size classes and a density fractionation is performed. This
procedure allows the manipulation of parameters such as
the grain and particle size so that there is some control over
the locking texture.
Work that has been done in this area is described below:
1. Bagga [11] created a standard material using 600-710
µm pyrite particles as the grain material and polystyrene as
the matrix. The locked blocks were crushed after treatment
with liquid nitrogen to make the polystyrene more brittle.
Several particle sizes were separated by screening and a
density fractionation was performed using CaCl2 and ZnCl2
solutions. A complete density fractionation could not be
performed since the highest density that could be reached
using these liquids is about 2 g/ml and the density of pyrite
is about 5 g/ml.
2. Woollacott and Valenta [12] embedded grains of a poly-
ester resin which had been doped with lead oxide powder
and black dye into a matrix of the same polyester resin in
liquid form, doped with white dye. The lead oxide powder
 A STANDARD MATERIAL FOR STEREOLOGICAL CORRECTION 123

Refinement of the standard material

Although artificial standard materials have been estab-
1. Embedding of monosize
lished, there are several parameters that can be changed to
grains into matrix.
enhance the quality and the quantity of the artificial stan-
dard material. The standard material could be improved by:

1. strengthening the bond between the grain and matrix

material. By producing a strong bond between the two
phases, there would be a decrease in breakage along the
interfaces and an increase in the amount of locked particles.
2. Grinding the grain-matrix The amount of locked particles produced should be sub-
blocks. stantial enough so that large amounts of grain and matrix
material do not have to be processed. In addition, strong
interfacial bonding would allow the standard material to
provide a test of models of liberation by size reduction.

2. changing the grain and/or matrix material. Ideally, the

phases for the standard material should be brittle so that
they are easy to crush and possess good polishing proper-
3. Size classification of the
ties so the interfaces are clearly delineated when viewed
particles
under a microscope. Also, the two materials should be sig-
nificantly different in density. The greater the difference in
density, the greater the resolution of the density separa-
tions. However, the density of the denser of the two phases
should not exceed the upper limit of the separation method.
4. Density classification.
3. creating other locking textures. With the current proce-
dure for producing locked particles, only granular locking
Fig. 1 Conceptual procedure for the production of artificial locked particles. can be created. While this may reflect the situation in many
ores, this is not necessarily always the case. For instance,
particles with a layered locking texture (a texture consist-
increased the density of the grain material to allow density
ing of alternating layers of different phases) may result if an
fractionation and the dyes provided optical differentiation
ore with a banded structure is crushed.
between the grain and matrix phases; this material was
designed for optical microscopy. When the matrix resin had
4. developing a strategy for producing only simple-locked
hardened, the locked blocks were crushed and screened to
particles. With the current procedure for manufacturing
2.5-4.0 mm. The separations were performed using a heavy
locked particles, simple locking can be produced only
liquid (ZnCl2 solution). The densities of the grain and
when the particle size is significantly smaller than the grain
matrix phases were 1.756 and 1.219 g/ml, respectively.
size, but this may seriously reduce the amount of locked
particles produced. In any case, it is very difficult to control
3. Lin et al. [13,14] created their standard material by
the amount of simple locking due to the granular nature of
embedding grains of silica in a matrix of epoxy resin. The
the texture: unless the grains are perfectly dispersed in the
silica density was 2.62 g/ml and the resin density was 1.22
matrix, grains that are close to each other will almost
g/ml. The particles were separated using sodium poly-
inevitably create complex locking (locking such that there
tungstate, a water-soluble heavy liquid. The particle size
is more than one interface between the phases in the parti-
was 75-106 µm.
cle). This is complicated by the fact that it is impossible to
measure the degree of simple locking since stereological
4. Gay [6] created a standard material in much the
bias affects the determination of the locking texture.
same manner as Woollacott and Valenta. Grains of a
polyester resin doped with zinc oxide powder and a
coloured dye were embedded in a polyester resin doped
RESULTS
with a different concentration of zinc oxide and a dif-
ferent coloured dye. The densities of the two phases
Selection of the phases for the standard material
were 1.36 and 1.62 g/ml. Two particles sizes, 2.36-2.80
mm and 3.35-4.00 mm, were generated by screening Two new materials were selected for the production of the
and separated using a ZnCl2 solution. standard material: lead borate (2PbO B2O3) as the matrix
•

material and glass particles as the grain material [7]. Lead

borate is a leaded glass additive and is more commonly

CANADIAN METALLURGICAL QUARTERLY

124 D. LIN and J.A. FINCH

used as a source of lead for glass melts or ceramic glazes, but 4. The power was shut off to the furnace and the crucible
in this work it was used as one of the phases of the standard was allowed to cool to room temperature.
material. The melting point of lead borate is approximately
500°C while the melting point of glass is approximately 5. The sample was removed from the crucible, crushed
800°C. The standard material was created by melting the lead and wet-screened to remove the fines.
borate and embedding the glass particles. The glass particles
softened slightly and produced a strong bond with the lead 6. The 425-600 µm fraction was screened out.
borate. (It was later determined that some glass diffused into
the borate which further strengthened the bond.) A SEM (scanning electron microscope) backscattered
electron micrograph of this material is shown in Figure 2.
Glass was used as the grain material because it has sim- A large majority of the sections exhibit locking. There were
ilar brittleness and breakage properties to lead borate. a few voids, but they were small (<10 µm) and were pre-
Silica was considered as the grain material, but the use of sent in only approximately 1% of the borate sections. It
glass rather than silica allows greater control over the lock- appeared that there were slightly more simple-locked sec-
ing texture (as seen by the creation of the layered texture tions than complex-locked sections. The complexity of the
discussed later) and because it has a lower melting point. complex-locked sections was low; most of the complex-
The density of the lead borate and glass were measured locked sections contained only two interfaces.
with a water displacement technique using a pycnometer
bottle [15] to be 6.833 g/ml (±0.006)1 and 2.502 g/ml
(±0.001), respectively. Subsequent experimentation showed
that after contact some glass diffused into the lead borate to
give a SiO2 content of 5.95% (±1.38%) as determined by
microprobe analysis. The density of the borate was re-
determined as 6.052 g/ml (±0.009) and this was the value
used in the density fractionation.

Due to the high density of the lead borate, convention-

al heavy liquids could not be used to fractionate the stan-
dard material so a Magstream Model 100, a centrifugal
magnetogravimetric separator, was used. (The principles of
the Magstream separator have been described by Walker,
Devernoe and co-workers [16,17,18,19].) The size range
for the standard material was selected as 425–600 µm since
600 µm particles are the largest that the Magstream Model
100 can accommodate and splits on the Magstream are
more precise the larger the particle size. 1 mm
1
Standard deviation in parenthesis
Fig. 2 SEM backscattered electron micrograph of 425-600 µm
glass/borate standard material particles taken at 30x magnification (light
phase is lead borate; grey phase is glass; dark phase is mounting medium).
Production procedure for standard material with a granu-
lar texture
The procedure for the creation of the glass/borate standard Production procedure for standard material with layered
material with a granular texture was as follows: texture and simple locking
1. Thirty grams of 1180-1700 µm glass grains were placed To create a standard material with a layered texture, alter-
in a 40 ml porcelain crucible. The glass was three Tyler size nating layers of the two phases were bonded together.
classes larger than the target particle size to aid in creating Simple-locked particles were created from this texture by
simple locking. crushing blocks of this material to a size below the thick-
ness of the layers as shown in Figure 3. The procedure for
2. Sixty grams of powdered borate was placed on top of the creation of the glass/borate standard material with sim-
the glass grains. Since the glass has a lower density than the ple locking was as follows:
borate, the glass will be wetted by the borate as it rises to
the top. 1. Long glass slides (75 mm x 25 mm x 1 mm) alternated
with short glass slides (25 mm x 25 mm x 1 mm) were
3. The crucible was placed in an induction furnace pre- clamped together at one end. This permitted the long glass
heated to 600°C. This temperature was maintained for 30 slides to be parallel to each other and separated by a gap of
minutes. exactly 1 mm.

CANADIAN METALLURGICAL QUARTERLY

 A STANDARD MATERIAL FOR STEREOLOGICAL CORRECTION
2. The slides were placed in a crucible containing borate
powder so that only the lower portion of the long slides was
in contact with the powder; the short slides and the clamp
itself were clear of the powder.
3. The crucible was placed in an induction furnace pre-
heated to 600°C. This temperature was maintained for 45
minutes.
4. The power was shut off to the furnace and the crucible
was allowed to cool to room temperature.
5. The clamp and the short glass slides were removed.
6. The sample was removed from the crucible, crushed
and wet-screened to remove the fines.
7. The 425-600 µm fraction was screened out.
Fig. 3 Simple-locked particles can be created if a layered-texture block
of material is crushed so that the particle size is smaller than the layer
thickness.
1 mm
Fig. 4 SEM backscattered electron micrograph of 425-600 µm simple-
locked, glass/borate standard material particles taken at 30x magnification
(light phase is lead borate; grey phase is glass; dark phase is mounting
medium).
125
A SEM backscattered electron micrograph of these par-
ticles is shown in Figure 4. Only simple locking was
observed; no sections with complex locking were seen.
The particle size of the simple-locked particles was
selected to be 425-600 µm because the granular-textured
standard material was this size. If the simple-locked and the
granular-textured standard materials were to be combined
to form a liberation distribution, the particles would have to
be the same size. Simple-locked and layered-texture parti-
cles are a useful supplement to the granular-textured stan-
dard material.
Density fractionation
To determine the liberation, the particles were separated
into different density classes using the Magstream separa-
tor. In this work, density fractionation was performed only
on the granular-textured standard material particles.
In common with all separators, separation on the
Magstream is not perfect. Also, Bunge and Fuerstenau
[20,21,22] observed that the accuracy of Magstream sepa-
rations decreases with particle size. A theoretical study by
Svoboda [23] concluded that the performance of the
Magstream was dependent upon particle size and he cau-
tioned against using the Magstream for fine particles. To
ensure separation accuracy, the heavies and lights products
must be re-processed (cleaned).
The density fractionation on the Magstream assumed
that the particles were non-magnetic. To verify this, the
magnetic susceptibility of the two phases of the standard
material was measured using a Frantz isodynamic magnet-
ic separator [24]. As expected, both the glass and lead
borate had very low magnetic susceptibility (κglass < 5.32 x
10-5 SI units and κlead borate < 1.95 x 10-5 SI units; for com-
parison, κchalcopyrite ≈ 4 x 10-4 SI units). Their diamagnetic
properties were also measured. Both materials showed no
measurable diamagnetism.
The standard material was separated with the
Magstream into the following composition fractions: -5, 5-
15, 15-25,..., 85-95, +95 vol.% borate. To ensure the accu-
racy of the separations, the following measures were taken:
1. The products of the first separation (rougher) were
cleaned twice. Therefore, for each composition fraction,
three separations were performed at both split-points of the
fraction.
2. In the cleaning steps, any particles that did not re-report
to the composition fraction were eliminated.
3. The split-points were set 0.5% closer to the midpoint of
the fraction. For instance, for the 45-55 vol.% borate frac-
tion, the split points were set to 45.5% and 54.5 vol.%
CANADIAN METALLURGICAL QUARTERLY
126 D. LIN and J.A. FINCH

borate. This leaves a 1% gap in composition between frac-
tions, but helps minimise misplaced particles.
The particles that were -5 vol.% borate or +95 vol.%
borate were considered to be free. True free glass particles
(i.e., 100% glass) were created simply by crushing glass to
425-600 µm. True free borate was created by placing borate
powder alone in porcelain crucibles and heating to 600°C
for 30 min. After the borate had cooled and solidified, it
was removed from the crucible and crushed to 425-600 µm.
Measurement of the grade of the composition fractions
Following Magstream separation, the grade (i.e., the per-
cent borate) of the composition fractions was determined.
Two different methods were used to measure the grade:
water displacement in a pycnometer bottle and image
analysis. Henceforth, the grade measured using these meth-
ods will be referred to as the pycnometer and IA grades,
respectively.
The IA grade is determined by microscopic examina-
tion of the particle sections. The total area of the two phas-
es is measured with an image analyser. It is known that the
area grade is not stereologically biased and is identical to
the volumetric grade [6(p.22)].
affects the IA grade. It is important to generate random sec-
tions. In these samples, the particles in each fraction should
have very similar densities and consequently, there should
be little segregation. But, regardless, precautions were
taken to ensure random mounting of the particles.
The sample preparation involved mixing 0.4 ml of the
sample with an equal amount of a diluent material (425-600
µm graphite particles) and placing the mixture at the bot-
tom of a 32 mm mold. The diluent helps to support the sam-
ple particles in space (and thus reduce preferential orienta-
tion and the incidence of particles touching) and promotes
random orientation [25]. Graphite was selected as the dilu-
ent since it has a low density and a grey level similar to the
mounting medium resin when observed by backscattered
electron imaging. The mounting medium was Epofix resin
(Struers Inc.). The resin was prepared by mixing with the
hardener and then centrifuging at 1600 rpm for 1 minute to
remove any air bubbles. A small quantity of the resin (0.8
ml) was added to the particles in the mold and mixed. The
small amount of resin helps inhibit preferential settling by
restricting the space in which the particles can move. The
mold was then centrifuged at 1600 rpm for 5 minutes to
remove any air bubbles that may have resulted from the
mixing. Afterwards, more resin was added to top off the
mold.

In sample preparation, prevention of preferential set- For the standard material, the pycnometer and IA grades
tling (due to density differences between the particles) and were measured for each composition fraction. The two
preferential orientation (due to density differences between grades should be close to the midpoint. The results are
the phases in the locked particles) is important since this shown in Table I.

Table I — Pycnometer and IA grades of the composition fractions of the standard material (density of borate,
6.052 g/ml; glass, 2.502 g/ml)

Composition fraction Magstream Pycnometer Pycnometer IA

(vol.% borate) split-points (g/ml) density (g/ml) grade (vol.% borate) grade (vol.% borate)

-5 -2.680 2.522 0.6 0.4

5-15 2.680-3.035 2.805 8.5 9.8
15-25 3.035-3.390 3.176 19.0 20.1
25-35 3.390-3.745 3.517 28.6 31.7
35-45 3.745-4.100 3.850 38.0 40.0
45-55 4.100-4.455 4.232 48.7 49.7
55-65 4.455-4.810 4.532 57.2 58.9
65-75 4.810-5.165 4.865 66.6 68.3
75-85 5.165-5.520 5.257 77.6 78.0
85-95 5.520-5.875 5.647 88.6 87.9
+95 +5.875 6.265 106.0 98.1

CANADIAN METALLURGICAL QUARTERLY

 A STANDARD MATERIAL FOR STEREOLOGICAL CORRECTION
For all the fractions, both the pycnometer and IA grades
fall in the composition fraction range and in most cases,
they are close to the midpoint of the range and the differ-
ences in grades are not significant.
The pycnometer grade of the +95 vol.% borate fraction
was greater than 100 vol.%. This can be explained by con-
sidering the creation of the standard material. Although the
glass is always in contact with the borate, there is a layer of
borate at the bottom of the crucible (the glass grains float in
the borate due to their lower density) that does not come in
contact with the glass. The borate density was calculated
only for borate that had been in close contact with glass
grains and where limited diffusion had occurred. All the
high density borate reports to the +95 vol.% borate fraction
where it belongs.
Use of the standard material
The standard material can be used to produce different lib-
eration distributions by combining the different composi-
tion fractions. These distributions can be used as a check on
the effectiveness of stereological correction procedures
provided the other components of liberation analysis - sam-
ple preparation and image processing - are performed cor-
rectly. The known true liberation distribution can be com-
pared with the corrected distribution. We have reported on
this comparison elsewhere [26]. In more general terms, the
standard material would enable the whole procedure (not
just stereological correction) to be tested, although the
source of error may be difficult to isolate. In this regard, a
standard material is superior to using computer-simulated
particles since it involves all the steps of a liberation analy-
sis. Since the two phases of the standard material are
strongly bonded to each other, the standard material can
also be used to test liberation models. Most of these mod-
els assume negligible breakage along grain boundaries.
CONCLUSIONS
A method was developed for the creation of a standard
material consisting of glass and lead borate. This standard
material is flexible and easy to use. Particles with granular
and layered textures were created along with particles
exhibiting simple locking. The standard material can be
used to test the steps in liberation analysis including stere-
ological correction procedures.
127
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