Int. J. Miner. Process.

84 (2007) 310 320

www.elsevier.com/locate/ijminpro

Modern SEM-based mineral liberation analysis

Rolf Fandrich , Ying Gu, Debra Burrows, Kurt Moeller
JKTech Pty Ltd, Isles Rd, Indooroopilly QLD 4068, Australia
Received 31 March 2006; received in revised form 24 July 2006; accepted 31 July 2006
Available online 5 October 2006

Abstract

Modern digital mine planning, plant design and mineral processing operations demand detailed characterisation of the ore and
plant feed. Textural parameters, such as mineral liberation size and mineral association, combine with modal mineralogy data to
strongly influence mineral processing conditions and recovery. Traditionally, the measurement of these ore characteristics
employed the tools of an optical microscope and/or a semi-automated SEM. These methods are time consuming, costly and
frequently produce semi-quantitative results from data sets that are too small to be statistically valid. Thus, the results cannot be
used reliably and effectively in digital mine planning and design.
In the last 10 years, modern SEM-based quantitative mineralogy tools have advanced rapidly with increasing computer power,
improved SEM hardware and the development of sophisticated image analysis methods. Texture resolutions can now be submicron
and SEM measurement times have reduced to less than an hour for simple analyses, where previously they required many hours.
Through image analysis, particle sections are recognised and separated, and the mineral grains within are delineated for discrete X-
ray analysis to determine mineralogy. The modern tools not only increase the speed and accuracy of liberation analysis, but also
enhance measurement automation. Automated standard collection assists with the setup of new ore types for routine analysis and
automated elemental quantification of target minerals enables the tracking of variations in the composition of the minerals of
interest.
The key to success for any modern SEM-based mineral liberation analysis system is the close integration of BSE image and
EDS X-ray analyses. Integration of the SEM-based quantitative mineral liberation analysis with optical microscope, dual beam
systems and X-ray tomography will further enrich the analysis results and the derived user experience.
2006 Elsevier B.V. All rights reserved.

Keywords: Scanning electron microscope; Mineral liberation analysis; Image analysis

1. Introduction fundamental parameters used for process plant design and

The significance and value of mineral liberation ana-
lysis to the subject of applied mineralogy and metallur-
gical processing has been well documented (Jones, 1987;
Petruk, 2000; King, 1993). Mineral liberation data are
Corresponding author. Tel.: +1 61 7 3365 5922.
E-mail address: r.fandrich@jktech.com.au (R. Fandrich).
0301-7516/$ - see front matter 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.minpro.2006.07.018
optimization. In recognition of this, several measurement
systems based on the application of scanning electron
microscope (SEM) technology to polished particles
sections have been developed (Hall, 1977; Pignolet-
Brendom and Reid, 1988; Jones, 1987; King, 1993;
Lastra et al., 1998; Petruk, 2000; Gu, 2003). The latest
advancement of such systems and the quality of the
mineralogical data being produced by them have
 R. Fandrich et al. / Int. J. Miner. Process. 84 (2007) 310320 311

ray measurements in a process to be known as particle

mapping.

2. Mineral liberation analyser

The JKMRC Mineral Liberation Analyser (MLA)

was first presented as a new development in the field of
SEM-based automated mineral measurement tools in
1997 (Gu and Napier-Munn, 1997). At the time it
represented a unique method of combining BSE image
analysis and X-ray mineral identification to provide
automated quantitative mineral liberation characterisa-
tion. The advanced analysis techniques implemented by
the MLA today are presented, as are the many methods
of combining them to provide targeted and optimised,
Fig. 1. Witwatersrand linear intercept measurement system.
automated mineralogical information.

extended their relevance upstream into the field of ore 2.1. BSE image analysis
characterisation for geological mapping purposes (Wil-
liams and Richardson, 2004). Imaging and image analysis are fundamental to
One of the earlier attempts to automate the gathering mineral liberation analysis. A low noise, high-resolution
of mineral liberation data from polished sections was image is a prerequisite for mineral identification and
undertaken by Peter King at Witwatersrand University quantification. The very stable BSE signals from a
(King, 1977). This system measured linear intercept modern SEM can generate quality high-resolution (0.1
lengths of the pyrite phase in a Witwatersrand quartzite 0.2 m) images of particle sections. These images allow
using an optical microscope. A mini computer con- the MLA, through its advanced image analysis techni-
trolled both a constant velocity motorized stage and a ques, to accurately discriminate the mineral phases
photometer circuit to register when the bright pyrite within a particle. The principal image analysis functions
phase moved under the lens (Fig. 1). used by the MLA are known as particle de-agglomer-
As is still the case today, the desired automation was ation and phase segmentation.
motivated by the need to find alternatives to the labour-
intensive manual viewing of sufficient particles to 2.1.1. Particle de-agglomeration
obtain a statistically significant set of data. The principle A liberation analysis using the MLA involves the
of applying thresholding to a signal generated by the setting of particles into a mould (typically 30 mm
reflectance of a mineral (here of photons) to achieve diameter) with epoxy resin to form a hardened block.
phase discrimination was also being applied to achieve Typical particle sizes range from 10 m to 1 mm and are
likewise with electrons in SEM-based systems such as
CESEMI (Troutmann et al., 1974).
The Mineral and Metallurgical Image Analysis
(MMIA) software developed at the University of Utah
(King and Schneider, 1993) applied thresholds to the
grey scale histograms from BSE images of polished
particle sections for phase discrimination (see Fig. 2).
MMIA allowed the automated batch processing of large
sets of high contrast and high-resolution images to
produce statistically reliable sets of both linear and areal
liberation data.
One of the first automated systems to intensively use
X-ray spectra was QEM SEM (quantitative evaluation
of materials by scanning electron microscopy) (Miller
et al., 1982). Digital images of particle sections where
built up in a pixel by pixel fashion by thousands of X- Fig. 2. MMIA software.
312 R. Fandrich et al. / Int. J. Miner. Process. 84 (2007) 310320

preferably of a defined narrow size fraction. The block is

then ground down to expose a representative cross-
section of particles which is subsequently polished and
then coated with carbon before being presented to the
SEM. Despite precautions to prevent it, inevitably some
particles in the prepared sample block will touch each
other. If not recognised by the system and treated
appropriately the agglomeration of particles can lead to
biased liberation results. The MLA system has an
automated de-agglomeration function that detects
agglomerates and separates them according to a set of
predetermined parameters. Fig. 3 shows this process.
The de-agglomeration function can be used both
during the on-line measurement or performed off-line. Fig. 4. Grey level distribution of a typical leadzinc ores. The x-axis is
Particle shape parameters determine if particles are the BSE grey level and the y-axis is the frequency.
agglomerated. The de-agglomeration procedure has
three methods or criteria at its disposal to find the
best separation option: 1) shadow or boundary identi- weighting applied to each of the separating criteria
fication, 2) linear feature recognition and 3) an erosion/ through a set of parameters. The adjustment of
dilation procedure. The operator can control the parameters may be needed to account for the influence

Fig. 3. MLA de-agglomeration process: (a) Original BSE image. (b) After background removal, several particles are agglomerated. (c) One of the
agglomerates is highlighted. (d) After de-agglomeration, the agglomerate is broken apart and one particle is highlighted.
 R. Fandrich et al. / Int. J. Miner. Process. 84 (2007) 310320
Fig. 5. BSE and segmented particle image.
on separation by varying particle characteristics such as
shape and size.
2.1.2. Phase segmentation
Once individual particles have been identified, the
next step of the liberation analysis identifies all distinct
mineral phases (or grains) and defines their boundaries
accurately. This process is called phase segmentation
and is performed on each individual particle. The MLA
phase segmentation function outlines the regions of
homogeneous grey levels within a particle BSE image.
The average BSE grey value of every defined region
corresponds with a mineral of unique average atomic
number (AAN). The AAN determines the number of
backscatter electrons emitted by the mineral and hence
is directly proportional to the grey level registered in the
BSE image. An example of a grey scale histogram with
its peaks corresponding to the minerals in a leadzinc
ore is shown in Fig. 4.
Phase segmentation also involves the recognition
and elimination of features of a BSE particle image
that do not represent an independent phase. These
Fig. 6. MLA area X-ray analysis of a composite particle.
313
artefacts can be cracks, shading, tiny voids or the
dark perimeter or halo that appears around many
particles.
The phase segmentation results for an enlarged BSE
image of a composite particle are shown in Fig. 5. Six
regions of homogeneous grey levels or mineral grains
have been identified. The segmented image is created
with each mineral grain in a particle being assigned a
unique colour.
In an ideal system and set of measurement conditions
each mineral within a sample will have a defined BSE
grey value. Should this grey level coincide with that of
another mineral, in the same particle, due to the same or
very similar average atomic numbers, as is the case for
pentlandite and chalcopyrite (AAN = 23.5), the MLA
resorts to another rendering method to be explained
later.
As particle-based segmentation uses the grey scale
histograms of each individual particle, the influence of
any grey level effects due to changes in measurement
conditions, such as beam drift, are eliminated.
2.2. Mineral identification with X-ray analysis
The MLA uses three X-ray analysis techniques to
identify mineral species: point X-ray, area X-ray and X-
ray mapping.
2.2.1. Point X-ray analysis
In a typical sample measurement the MLA performs
one X-ray analysis (typically N 2000 counts) for each
grey level region identified within a segmented particle.
The spectrum is collected at the centre of a phase to
314 R. Fandrich et al. / Int. J. Miner. Process. 84 (2007) 310320
avoid contamination from bordering phases and hence
acquire the cleanest spectrum possible. This spectrum
is linked to its corresponding particle and grain in the
segmented image to generate what is known as an X-ray
image. The stored spectra are then compared with a
predefined list or library of standard mineral spectra to
complete the identification procedure and produce a
classified image. In the classified image in Fig. 6 four of
the five delineated phases were identified as chalcopy-
rite and the other as bornite. The classified image, and
specifically the pixel phase data contained within, is the
basis for all further quantitative analysis. In addition to
particle location data, the pixel data and related mineral
characteristics are stored in a database for subsequent
presentation using the MLA software: DataView.
2.2.2. Area X-ray analysis
During area X-ray analysis the spectra are collected
by rastering the beam over the phase area. The perimeter
of the phase is not scanned to avoid contamination by
adjoining phases. Area X-ray analysis can be imple-
mented where there is the possibility of two or more
associated minerals having the same AAN (i.e.
associated pentlandite and chalcopyrite grains). Poor
BSE grey level contrast can result in two phases not
being segmented and hence no delineation of phase
boundaries (see Fig. 7, top left). With point X-ray
analysis, depending on which mineral happens to be at
the point of X-ray collection, the resulting combined
phase will be identified as either pentlandite or
chalcopyrite. Area X-ray analysis detects that two or
Fig. 7. Illustration of X-ray mapping for a particle containing pentlandite and chalcopyrite.
more phases are present through the resulting mixed
spectra. X-ray mapping can then be employed to
identify the mineral phases and to resolve the phase
boundaries.
2.2.3. X-ray mapping
X-ray mapping imposes a grid over an entire particle
image, or specific grains thereof, and collects X-ray data
at each grid point to determine the mineral identity. Fig. 7
illustrates the procedure with the example of pentlandite
and chalcopyrite. Mineral identification using mapping
requires significantly more time (greater than one order
of magnitude) than point and area X-ray analysis as
many more spectra are collected to generate a compre-
hensive mineral map.
The three fundamental X-ray analysis methods of
point and area X-ray analysis and X-ray mapping are the
building blocks of all MLA measurement modes
involving X-ray identification.
2.2.4. Mineral standards library
Mineral identification through X-ray analysis
requires a library of mineral standards. This library is
usually constructed before an automated run and
involves the collection of a high quality X-ray spectra
spectrum for each mineral in the sample. The building of
a standards library directly from the sample ensures that
measurement conditions are reflected in the standards,
such as beam energy (i.e. keV), and it also provides for
an elemental deportment that better reflects the
chemistry of the sample.
 R. Fandrich et al. / Int. J. Miner. Process. 84 (2007) 310320
The spectra identification process involves an error-
based search for the measured spectrum in the standards
library to find the most probable fit. Statistics on the
spectral pattern matching can be examined to assess the
confidence of classification for specific minerals.
2.3. MLA measurement modes
The many measurement modes offered by the MLA
implement the fundamental BSE image, and the various
X-ray analyses to produce a suite of measurements
designed to accommodate many different mineralogical
information requirements. The measurement types and
their applications are described.
2.3.1. Standard BSE liberation analysis (BSE)
This is the most basic liberation analysis method in
which a series of BSE images are collected on-line and
then processed off-line to produce liberation data.
Mineral discrimination is based solely on BSE grey
level contrast and the liberation data is generated
exclusively through image analysis. BSE is employed
for applications where good grey level contrast exists
and a correlation between grey level peak and mineral
species is established. This is the case for certain lead/
zinc and copper ores and some slags. BSE is also useful
for textures or features that are finer than the resolution
of X-ray analyses (i.e. 25 m).
Fig. 8. Illustration of a GXMAP analysis.
315
2.3.2. Extended BSE liberation analysis (XBSE)
XBSE implements area X-ray analysis to efficiently
and effectively analyse ore samples containing phases
with sufficient BSE contrast to ensure effective
segmentation. The high resolution of BSE imaging for
grain boundary definition and the speed of single X-ray
mineral identification make this method ideal for a great
majority of mineralogical samples.
An extension of this mode is XBSE with automated
standards collection (XBSE_STD). If a spectrum from a
particular phase cannot be identified using the existing
library of standards, a standard for the unknown phase
will be collected in the usual manner and added to the
library for later classification.
2.3.3. Ford analysis or grain-based X-ray mapping
(GXMAP)
GXMAP employs X-ray mapping to the phases that
cannot be segmented by BSE grey levels alone and the
employs the faster area X-ray analysis for phases that are
readily segmented. The operator selects the grains for
mapping through a BSE trigger or a specific X-ray
standard trigger. Fig. 8 illustrates the advantages of the
selective mapping of GXMAP over traditional X-ray
mapping for the example of a particle containing
pentlandite, chalcopyrite and quartz. A BSE trigger set
at a grey level below that of pentlandite and chalcopyrite
ensures that all grains of interest are mapped, saving
316 R. Fandrich et al. / Int. J. Miner. Process. 84 (2007) 310320
valuable measurement time. Alternatively the X-ray
standards for pentlandite and chalcopyrite can be
implemented to trigger the mapping. A series of mixed
spectra, interpolated at 10% intervals between the
nominated pure pair of spectra, is generated and
compared with the mixed spectra measured by the
area X-ray analysis to force the trigger.
GXMAP is a flexible mapping technique an advance-
ment on the older MLA mapping methods of particle X-ray
mapping (PXMAP) and selected particle X-ray mapping
(SXMAP) (Gu, 2003). It has been successfully applied to
certain types of sphalerite and chalcopyrite as well as
textually complex ores, such as nickel ores containing
pentlandite as fine flames in pyrrhotite. This mode is
named after its co-developer Dr. Fred Ford (INCO).
2.3.4. Sparse phase liberation analysis (SPL)
This measurement mode searches BSE images for
particles containing phases of interest using a BSE grey
scale range and then performs an XBSE analysis on them.
The off-line processing is identical to the XBSE method
and generates the same mineral liberation and association
data. It does not provide bulk mineralogy information, as
only selected particles in the sample are analysed. The
selectivity of the SPL measurement is designed to effi-
ciently measure tailings and low grade feed ores, such as
platinum group mineral (PGM) ores where the mineral
associations of the phase of interest is of importance.
Two specialised versions of SPL analysis are also
available. SPL-Lite (SPL-LT) only measures the sparse
Fig. 9. Gold found by the RPS mode.
phase of interest and its external mineral associations.
This is appropriate for rock mass applications, such as
drill cores, where liberation data is not relevant.
SPLMAP maps the internal associations of the phase
of interest once found or can be described as a GXMAP
applied to a SPL.
2.3.5. X-ray modal analysis (XMOD)
XMOD is the classical point counting method in
which mineral identification is determined by one X-ray
analysis at each counting point. This mode uses BSE
imaging to discriminate particle matter from back-
ground and then collects one X-ray spectrum from each
grid point across the particle. The X-ray spectra are
saved for off-line classification. This method only
produces modal mineralogy information, i.e. percen-
tages of the mineral components of the sample.
XMOD can also be implemented to produce a line
scan measurement mode that produces traditional linear
intercept data. X-ray spectra are taken at a step size of
one pixel in the x direction and a given y displacement
determines the line spacing.
2.3.6. Rare phase search (RPS)
The RPS mode searches the BSE images for phases
of interest using a trigger and collects a corresponding
characteristic X-ray spectrum. For each grain found, the
system saves the image of the particle containing the
grain, the stage location and its X-ray spectrum. The
operator can subsequently move to the SEM stage
 R. Fandrich et al. / Int. J. Miner. Process. 84 (2007) 310320
location where the grain was located and manually
investigate it and its surroundings further. RPS is
designed to efficiently locate very fine (sub-micron)
components in large particle populations, such as gold in
tailings and deliver data such as grain size and
associated minerals (see Fig. 9). The ability to classify
off-line allows the operator to automatically eliminate
other bright phases, such as galena, from the phases of
interest.
2.3.7. Latti analysis (SXBSE)
The Latti measurement mode adds an elemental
quantification capacity to the XBSE analysis and is also
known as a Super XBSE analysis. An X-ray standards
trigger is employed, in a similar fashion to the GXMAP
mode, to initiate a so-called long count X-ray analysis.
This X-ray collection can last 20 s or more and contain
up to over 1,000,000 counts and is comparable with a
high quality quantitative EDS measurement of the
mineral concerned. These long count spectra are stored
separately for subsequent analysis to obtain accurate
elemental quantification for the minerals of interest,
such as those with variable stoichiometry e.g. sphalerite.
Fig. 10. MLA data presentation software: DataView.
317
This mode is named after its co-developer Dewetia Latti
(Rio Tinto).
2.3.8. Schouwstra analysis (SPL-dual zoom)
Here, a standard SPL analysis is performed and when
a phase of interest is detected in an image, the image
capture is repeated at a higher resolution. The SPL
analysis is then performed for the higher resolution
particle images. This measurement mode combines the
advantages of a rapid search for the phase of interest at
low resolution (typically 1024 800) and that of
accurate imaging at a high resolution (up to
4096 3200). Schouwstra analysis is widely used for
PGM minerals and is named after its co-developer Dr.
Robert Schouwstra (Head of Mineralogical Research,
Anglo Platinum).
2.4. MLA data presentation
DataView is the data presentation software that
enables the operator to examine, process, present and
store the quantitative mineralogical data generated by
the MLA measurement software. Pixel data is combined
318 R. Fandrich et al. / Int. J. Miner. Process. 84 (2007) 310320

Fig. 11. Mineral grouping and corresponding grade recovery curves.

with the elemental composition and densities of the
identified minerals to produce a variety of mineralogical
data: modal mineralogy, calculated assay, elemental
distributions, elemental and mineral grade recoveries,
particle and mineral grain size distributions, particle
density distributions, mineral associations and locking,
phase specific surface area (PSSA) and mineral
liberation by particle composition and free surface.
Both tabular and standard graphical representations of
the data are available (see Fig. 10). The combination and
comparison of data sets are possible, as well as the
ability to select particle populations through filtering
and to manage mineral lists via grouping.
2.4.1. Filtering
Filtering enables the creation of subsets of a particle
population stored within a particle database according to
given criteria. The criteria currently available are
filtering by particle size, density, and shape, as well as
mineral and elemental weight composition. For example
a filter of density N 3.0 would create a subset of all
particles with a calculated density of greater than 3.0.
All the analyses offered by DataView can then be
performed on this subset.
2.4.2. Grouping
As the list of minerals identified by an MLA analysis
can be extensive and can contain many minor minerals of
little consequence to an analysis, a grouping function
allows mineral groups to be defined and be further treated
as an individual mineral phases. Fig. 11 illustrates how the
copper sulphides in a mineral list have been grouped and
used to display the theoretical grade recoveries of three
measured size fractions in a feed sample.
3. Future developments
The goal of ongoing MLA development activities is
to provide improved and diverse mineralogical infor-
mation through the provision of advanced analysis tools

Fig. 12. Fusion of images from light microscopy and SEM.

 R. Fandrich et al. / Int. J. Miner. Process. 84 (2007) 310320
and high levels of measurement automation. The
generation of mineralogical information from measure-
ment data is enhanced through linkages with simulation
tools. Levels of measurement automation are improved
by integration with other measurement systems and
technologies.
3.1. Links with simulation
Commercial software packages designed to simulate
mineral processing operations provide valuable optimi-
sation and design tools for plant metallurgists and
require reliable, quantitative mineralogical data to
deliver meaningful results. Establishing efficient links
between simulation and measurement tools increases the
value of the information derived. For example, flotation
models can utilise particle grade and mineral liberation
distributions to predict and optimize grade recovery
curves for flotation circuits. Linkages of this nature
contribute to the goal of upgrading mineralogical data to
metallurgical information for decision making.
3.2. Integration with optical microscopy systems
Materials with predominately organic components
and hence with very low atomic numbers, such as coal,
are not conducive to liberation analysis with electron
microscopy systems. Light optical microscopy systems
such as MACE300 (Jenkins et al., 2004) offer
solutions to characterising coal particles based on the
light reflectance and texture of the organic phases or
macerals. Combining the identification and phase
discrimination capabilities of both measurement princi-
ples through image fusion techniques can offer
comprehensive liberation analysis solutions for coal,
incorporating both maceral and mineral matter (Fig. 12).
Previously unattainable detailed maceralmineral asso-
ciation data can provide new information for process
optimisation, the prediction of coal utilisation perfor-
mance and the definition of new coal quality levels.
3.3. 3D mineral analysis
The topic of stereological correction in mineral
liberation analyses has been examined extensively and
various models for extrapolating 3D liberation results
from 2D particle section measurements have been
proposed and reviewed (Latti and Adair, 2001). An option
to apply such methods to measured liberation distributions
will be offered by future versions of DataView.
Pioneering 3D liberation measurement studies on
materials such as a sphalerite/dolomite ore and coal
319
using X-ray computed tomographic (CT) techniques at
the University of Utah have been reported by Miller and
Lin (2004). The combination of MLA analysis with the
ion beam milling and deposition capability of a dual
beam SEM system (Quanta 3D system offered by FEI)
will similarly enable the direct measurement of 3D
mineral liberation data. Through serial sectioning with
subsequent repeated MLA analysis, a tool for undertak-
ing automated 3D quantitative mineral liberation
analyses will be available.
4. Conclusion
Prudent use of both BSE and X-ray signals from an
SEM to exploit their advantages, in conjunction with
advanced image and pattern recognition analysis, are the
keys to success for a modern automated SEM-based
mineral liberation analysis system. The speed of
acquisition and the high resolution nature of BSE
imaging are combined with the accurate mineral
identification capabilities of X-ray analysis in such a
way to optimise an MLA analysis to the requirements of
specific samples and applications. The eight basic MLA
measurement modes vary from a purely BSE-based
technique (BSE method) through to an almost exclu-
sively X-ray analysis point counting technique
(XMOD).
In addition to a high level of automation, the modern
MLA system has achieved speed, resolution, versatility
and accuracy. The current levels of automation extend
from de-agglomeration functions to the ability to probe
unidentifiable phases (Latti method) and to recognise
mixed spectra (standards trigger). Future linkage and
integration developments will provide for a new de-
finition for a modern SEM-based mineral liberation
analysis.
Acknowledgements
The authors acknowledge the work of the entire
MLA group at JKTech. The contributions of program-
mers to software development and those of analysts to
measurement methodology development have been
invaluable.
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