CHAPTER 1: USE OF THE MINERAL LIBERATION ANALYZER (MLA) FOR MINERALOGICAL

STUDIES OF SEDIMENTS AND SEDIMENTARY ROCKS

Paul J. Sylvester,
Department of Earth Sciences, Memorial University,
St. Johns NL, A1B 3X5
E-mail: psylvester@mun.ca
for quantitative mineralogy developed in 1970s
(Troutmann et al. 1974, Grant et al. 1976, Hall
1977); the QEM*SEM (Quantitative Evaluation of
Mineralogy by Scanning Electron Microscope)
technology developed by CSIRO Minerals,
Australia, in the 1980s (Miller et al. 1982, Reid et
al. 1984, Pignolet-Brendom & Reid 1988); the MP
SEMIPS (MicroProbeScanning Electron MicroscopeInduced Photoelectron Spectroscopy) image
analysis instrument developed by CANMET,
Natural Resources Canada, also in the 1980s (Petruk
1987, 1989); and the Mineral and Metallurgical
Image Analysis software developed at the
University of Utah in the early 1990s (King &
Schneider 1993). Besides the MLA, the other
commercially available automated SEM system for
mineral analysis is the QEMSCAN instrument
(Butcher et al. 2000, Gottlieb et al. 2000, Pirrie et
al. 2004), which is based on the QEM*SEM
technology, and is also sold by FEI Company. In
addition, a notable system for CCSEM (Computer
Controlled Scanning Electron Microscopy) has
operated at the Geological Survey of Denmark and
Greenland (GEUS) since the mid 1990s (Knudsen
1998, Keulen et al. 2012).
Application of the MLA system was focused
initially around applied mineralogy and
metallurgical processing (Fandrich et al. 2007), in
particular on determining the degree of liberation of
ore minerals from gangue (e.g., Ford et al. 2011,
Kelvin et al. 2011); hence the origin of the name
mineral liberation analyzer given to the
instrument. More recently the potential of the MLA
has been recognized for other applications including
studies of sediments and sedimentary rocks such as
heavy mineral provenance (Lowe et al. 2011,
Tsikouras et al. 2011); microstructures in mine
tailings (Redwan et al. 2012); and till and stream
sediment prospecting (Wilton & Winter 2012). This
chapter illustrates some of the capabilities of the
MLA for mineralogical studies of sediments and
sedimentary rocks.

INTRODUCTION
The Mineral Liberation Analyzer (MLA) is a
scanning electron microscope (SEM) equipped with
energy dispersive X-ray (EDX) spectrometers, and
computer software that automates microscope
operation and data acquisition for automated
mineralogy. Various quantitative data sets including
modal mineralogy, porosity, grain size and shape,
mineral associations and digital textural maps are
collected on polished surfaces of rocks, sediments
or other particulate samples. MLA measurements
are based on backscattered electron (BSE) image
analysis for determining grain boundaries and
locations for X-ray spectral acquisition, and
classification of the characteristic X-ray spectra of
mineral species by comparison to a library of
reference spectra.
Advantages of the MLA for mineralogical
investigations over traditional optical microscopy
alone are: (a) the replacement of tedious manual
analysis by systematic, computer-automated
analysis, reducing the potential for operator bias and
human error; (b) the increased through-put and the
number of mineral grains examined, providing a
more statistically representative analysis of a
sample; and (c) the ability to distinguish finegrained or complexly intergrown minerals at the
scale of micrometres. Disadvantages of the MLA
are: (a) the difficulty of distinguishing minerals with
very similar compositions (e.g., gypsum and
anhydrite); (b) the inability to distinguish
polymorphs (e.g., calcitearagonite; rutileanatase
brookite; kyanitesillimaniteandalusite); and (c)
the lack of widely available standard reference
materials to demonstrate accuracy and precision of
results.
The MLA instrument was developed at the
Julius Kruttschnitt Mineral Research Centre
(JKMRC) of The University of Queensland,
Australia, in the mid 1990s (Gu & Napier-Munn
1997, Gu 2003). It became available commercially
in 2000, and is now marketed by FEI Company. The
design is built on automated electron beam systems

Mineralogical Association of Canada Short Course 42, St. Johns NL, May 2012, p. 1-16

USE OF THE MINERAL LIBERATION ANALYZER FOR STUDIES OF SEDIMENTS AND SEDIMENTARY ROCKS

beam excitation energy. Typical operating

conditions use an accelerating voltage of 25 kV and
beam currents of 1015 nA. X-ray measurements
are ultra-fast, up to 200 per second. The smallest
practical particle size that can be identified and
mapped by the MLA software is 0.2 m, although,
at such sizes, host minerals can sometimes create
problems with recognition and spectral
interferences. The SEM of the MLA is available as
either a conventional W filament or Field Emission
Gun (FEG) source system. The FEG produces an
electron beam that is smaller in diameter, more
coherent and up to 1000 times brighter than
W-tipped filaments. This results in improved signalto-noise ratio and spatial resolution. The intrinsic
SEM imaging resolution is 1.2 nm for the FEG
source, compared to 3.0 nm for the thermal, W
hairpin source (FEI Company 2012).
Samples for the MLA need to be presented as
flat, polished surfaces, coated with a thin conductive
film, usually carbon. Although the Quanta SEM can
image non-conductive specimens without carbon
coating in low vacuum, high pressure environmental (ESEM) mode, EDX analysis gives poor
results at high pressures and the MLA software does
not integrate ESEM information. Particulate
samples such as sediments are normally mounted in

INSTRUMENTATION
The SEM generates a beam of electrons in a
vacuum (usually 105 mbar or better) that is focused
by a series of electromagnetic lenses separated by
apertures in the electron column and scanned in a
raster pattern over a specific area of the rock or
sediment sample. The scanned area is called a
frame; decreasing the size of the frame (increasing
the magnification) increases the frame resolution.
Backscattered electrons reflected off the minerals in
each frame are collected on a screen to produce an
image. Electrons that interact with the minerals
generate X-rays with measured energy levels that
are characteristic of the elements present. The MLA
software for automated mineralogy integrates the
images and X-rays to identify the minerals and map
their distribution in the frame, and then steps the
SEM beam to the next frame where the
measurements are repeated.
As currently configured by FEI Company,
the MLA is based on a Quanta SEM platform, fitted
with dual, liquid nitrogen-free, SDD-type (Bruker
XFlash silicon drift detector, energy resolution:
133 eV) EDX spectrometers, a BSE detector and a
secondary electron detector (Fig. 1-1A). Some older
instruments employ Si(Li) liquid nitrogen-cooled
detectors. The SEM provides up to 30 kV electron

Figure 1-1. Components of the MLA instrument: (A) location of the EDX and secondary electron detectors, the electron gun
and column, and sample chamber on the Quanta 650 FEG SEM; views inside the sample chamber, showing the sample
holders for (B, next page) 30 mm round epoxy particle mounts and (C, next page) 27 x 46 mm petrographic thin sections.
Photo credit: Lauren Flynn.

P.J. SYLVESTER

Figure 1-1. Components of the MLA instrument: views inside the sample chamber, showing the sample holders for (B) 30
mm round epoxy particle mounts and (C) 27 x 46 mm petrographic thin sections. Photo credit: Lauren Flynn.

polished epoxy rounds. The standard sample holder

accepts either 8 or 14 round, 30 mm diameter (25
mm diameter with insets) epoxy mounts (Fig. 1-1B).
There are also standard holders for polished
petrographic thin sections of rocks (Fig. 1-1C) and
rock slabs. Other holders may be customized for
specific sizes of samples of interest, limited only by
the size of the vacuum chamber.

SAMPLE PREPARATION
Petrographic thin sections of rocks can be of
normal thickness (30 m) or thicker (100 m), if
additional material is needed for laser ablation (see
Koler 2012, Chew & Donelick 2012) or other
destructive micro-analytical techniques that might
be employed following MLA measurements. Epoxy
mounts of sediments or crushed sedimentary rocks

USE OF THE MINERAL LIBERATION ANALYZER FOR STUDIES OF SEDIMENTS AND SEDIMENTARY ROCKS

are made after sieving the particles into discrete size

fractions, typically 63 to 125 m (230 to 120 mesh),
125 to 177 m (120 to 80 mesh), 63 to 177 m (230
to 80 mesh), or 177 to 354 m (80 to 45 mesh),
depending on sieve sizes available, and goals of the
study. (In MLA terminology, particles are the
sieved objects that are mounted and grains are the
discrete mineral objects that make up the particles.
A particle can be composed of just one mineral
grain, or many.) In order to minimize biases
associated with non-representative sampling, riffling
and sub-sampling prior to mounting is important
(Petersen et al. 2004).
Particles larger than 500 m are not normally
mounted because comparatively few particles could
be included in the mount, and it would be unclear if
they would be statistically representative of the size
population. (That said, some analysts would prefer
to analyze a very coarse-grained particle section
rather than a rectangular thin section because
randomly oriented particles in an epoxy mount
would still be more representative of the sample
than a single thin section.) Particles smaller than
about 15 m pose practical problems for mounting
because of possible bias due to particle loss during
sieving and polishing. Where there is concern that
conventional mechanical crushing of samples will
fracture a significant proportion of mineral grains
resulting in a biased distribution of their size and
shape, electric pulse disaggregation (EPD; Cabri et
al. 2008) may be used instead. EPD applies a series
of high voltage electric shocks to a sample placed in
a water bath, which preferentially liberates mineral
grains by fracturing along grain boundaries.
When making mounts, a low viscosity resin
may be used to enable particles to preferentially
settle with their largest face parallel to the surface of
the mount so that size and shape measurements of
elongate particles are not biased by variable orientations (e.g., Tsikouras et al. 2011). Alternatively, if
there is a large variation in mineral density in the
sample and bias associated with density stratification in the mount is suspected (e.g., for placer Au
grains in a stream sediment sample), monolayer
particle mounts may be made. For monolayers, the
particles are spread out on a piece of double-sided
sticky tape attached to a flat surface over a circular
area 25 or 30 mm in diameter. Particles not adhering
to the tape are removed by gently tapping them off
before the mold is attached and the epoxy is poured.
For studies of minor to trace heavy minerals
in sediments or sedimentary rocks (see Morton
2012, Keulen et al. 2012, Koler 2012, Chew &

Donelick 2012, Pe-Piper & Piper 2012), the sample

may be concentrated to increase the numbers of
heavy mineral grains available for mounting and
analysis. This may be accomplished by using heavy
liquids such as bromoform (CHBr3; 2.889 g/ml),
methylene iodide (CH2I2; 3.325 g/ml) or non-toxic,
water-based LST (Li polytungstate solids that can
be used at any density up to 2.95 g/ml by diluting
with water). In this approach, the sieved samples are
added to a separatory funnel containing the heavy
liquid and the minerals of interest, which are denser
than the liquid, sink to the bottom of the funnel
under gravity and are recovered (Fig. 1-2A). An
alternative method called hydroseparation produces
heavy mineral concentrates of particles after settling
in a controlled upward pulsating water flow (Fig.
1-2B,C). The pulsating water flow limits the settling
of large, less dense particles, but allows smaller,
denser particles to settle unhindered, increasing the
efficiency of separation compared to passive gravity
settling alone (Rudashevsky et al. 2002, Cabri et al.
2006).
MLA MEASUREMENTS
Analysis Sequence and Run Times
The MLA software provides several
measurement methods but the two most commonly
used are referred to as XBSE and GXMAP.
XBSE is a versatile mode for particle mounts, where
all mineral grain boundaries are discriminated
simply by BSE imaging, and a single X-ray analysis
for each grain is used to verify mineral
identification. GXMAP is usually the most
appropriate mode for petrographic thin sections,
where it is likely that the grain boundaries between
two or more important minerals such as albite and
quartz have very similar BSE brightness and cannot
be distinguished without the use of detailed X-ray
analysis on a grid pattern, a process referred to as
X-ray mapping. In both cases the SEM collects
BSE images and X-ray data for a series of frames by
stepping across the particle mount (Fig. 1-3A) or
thin section (Fig. 1-3B).
The number of frames measured for a sample
can be set by the operator, or limited by a stated
time allowed for the analysis of the sample or a
required number of particles to be measured. A
typical run time for an XBSE analysis of a particle
mount is less than about 3 hours (barring a need for
high resolution imaging), covering approximately
100150 frames, each 1.5 x 1.5 mm, with a typical
resolution of 800 x 800 pixels. (Frame sizes are
dependent on particle sizes. It is desirable to

P.J. SYLVESTER

Figure 1-3. Typical analytical traverse of frames analyzed

by the MLA for (A) particle mounts and (B)
rectangular petrographic thin sections. For the particle
mounts, the measurement starts in the center of the
block and moves in a clockwise pattern. For the thin
section, the measurement starts from the bottom left
and moves across and up the slide.

Figure 1-2. Laboratory set-ups for two approaches for

heavy mineral concentration of rocks and sediments to
be presented to the MLA using: (A) heavy liquids in
separatory funnels, and (B) hydroseparation, with (C)
a close-up of the glass separation tube. Photo credits:
(A) David Lowe, and (B, C) Louis Cabri.

USE OF THE MINERAL LIBERATION ANALYZER FOR STUDIES OF SEDIMENTS AND SEDIMENTARY ROCKS

measure ~100 particles in a frame; therefore frame

sizes typically range from 12 mm depending on
particle size.) Using these parameters, some 10,000
to 20,000 particles will be analyzed for finer grained
fractions (e.g., 63 to 177 m) and some 5,000 to
10,000 particles for coarser grained fractions (e.g.,
177 to 354 m). A typical run time for a GXMAP
analysis of all mineral grains in a 27 x 46 mm thin
section is about 6 hours (for an SEM with a
conventional W filament source SEM) or 2.53
hours (for an SEM with a FEG source), covering
approximately 250300 frames, each 2 x 2 mm,
with a resolution of 400 x 400 pixels. For this case,
the primary spatial resolution from BSE imaging
would be 5 m, whereas the secondary resolution is
relative to the defined size of the X-ray mapping
grid, which is typically ~50 m, based on a 10 pixel
GXMAP step size.

In XBSE analysis, the identity of the

segmented mineral grain is further assessed by a
single X-ray analysis, either a scan over a defined
area or at a single point at the geometric center of
the grain (Fig. 1-5A). For GXMAP analysis, a
closely spaced grid of X-ray measurements is made
over the entire particle of interest (Fig. 1-5B).
Because X-ray mapping extends run times and
slows throughput of the instrument, it may be
triggered in GXMAP only for grains that have
particular greyscale values or X-ray spectra that are
known to be difficult to classify as particular
mineral species. For example, albite and quartz have
very similar average atomic number Z (10.7 vs.
10.8, respectively) and values (0.1255 vs. 0.1268,
respectively) (Fig. 1-4) and thus cannot be
distinguished by BSE-imaging alone. For thin
sections, however, which typically contain minerals
with similar Z values intergrown at a variety of
scales, X-ray mapping is typically set to trigger for
grains with almost the entire range of BSE
brightness (e.g., 30255).
Mineral classification by X-ray analysis is
based on matching the entire spectrum of energy
peaks collected on an unknown mineral to a library
of X-ray spectra for known reference minerals
collected using the same instrument parameters
excepting acquisition time. (Reference spectra
typically contain 10,000 counts, whereas unknown
spectra will typically have between 2,000 and 8,000
counts. This is because longer dwell times are used
for the reference spectra, where precision is most
important, than for unknown spectra, where dwell
times are set with respect to analytical speed.) X-ray
spectra on additional reference materials may be
collected to expand the library. The MLA software
compares the spectrum of the unknown to each
reference standard in terms of peak position, peak
shape and intensity ratios using a chi-squared
difference test on all channels in the spectrum. The
reference standard with the highest probability of a
match identifies the unknown mineral, with a
probability value (0100%) shown. Where the
probability is less than 80%, it is advisable to
consider collecting spectra on additional reference
standards. For each MLA project, compositions of
examples of each unknown mineral in the sample
should be characterized by wavelength dispersive
X-ray (WDX) analysis using an electron
microprobe, particularly for minerals known to
exhibit extensive element substitutions. The peak
resolution of WDX spectrometers is more than ten
times better than that of EDX spectrometers

Image Analysis and Mineral Identification

For both the XBSE and GXMAP methods,
the analysis begins with the delineation of the
boundaries between different mineral grains based
on brightness contrasts in the BSE images of each
frame. The backscattering coefficient is the
number of electrons backscattered by a mineral
(NBSE) relative to the number of incident electrons
from the SEM (NIE) where,
= NBSE NIE

(1)

and is a function of the average atomic number (Z)

of the mineral (Heinrich 1966) (Fig. 1-4),
= 0.0254 + 0.016 Z
0.000186 Z2 + 8.3107 Z3 (2)
Minerals composed of heavier elements (e.g.,
zircon) backscatter more of the incident electrons of
the SEM (have a higher value) and appear
brighter in the BSE image, whereas minerals
composed of lighter elements (e.g., quartz)
backscatter fewer electrons (have a lower value)
and appear darker. The MLA acquires BSE data as a
256 level grey scale image (0 = black, 255 = white)
and relates the value for each mineral to a range of
greyscale values between 0 and 255. The greyscale
variations in the BSE images collected by the MLA
provide a very rapid and effective method of
distinguishing boundaries between mineral grains
(a process referred to as segmentation in the
MLA software) while the grey scale values
themselves provide a first order identification of the
mineral.

P.J. SYLVESTER

Figure 1-4. (A) Average atomic numbers (Z) for some common minerals found in sediments and sedimentary rocks and (B)
the relationship of mineral Z with the proportion of backscattered electrons produced from a given incident electron beam.
The red circles along the curve are the same minerals as in (A) with particular minerals identified as blue boxes.

USE OF THE MINERAL LIBERATION ANALYZER FOR STUDIES OF SEDIMENTS AND SEDIMENTARY ROCKS

Figure 1-5. Schematic illustration of MLA measurements made in (A) XBSE and (B) GXMAP modes. In both cases, BSE
contrast delineates multiple grains in the particle. In XBSE mode, an EDX analysis is made at a single point in the grains in
the segmented image, which reveals that only two minerals are present, and their distribution is defined and proportions
calculated. In the case of GXMAP, the entire particle is mapped in detail using a grid of EDX analyses in order to define
the minerals present and their proportions.

(~10 eV compared to ~133 eV) and so closely

spaced peaks can be measured more precisely and
identified more accurately. The same mineral grains
in the sample analyzed by WDX on the electron
microprobe can be also analyzed by the MLA and
added to the MLA reference library to ensure more
accurate matching to the unknowns.

DATA OUTPUTS
The data products of an MLA analysis are
false color digital images of each frame, coded by
mineral species, showing the texture of the sample,
and linked to BSE images and quantitative data for
each particle and grain. Each of the frames analyzed
in a particle mount or thin section may be stitched

P.J. SYLVESTER

radius of an equivalent area ellipse. The angularity

value increases with increasing surface roughness.

together using the MLA software to produce a

larger mosaic of the sample. The software provides
a program (called MLA Image Processing) for
examining the BSE and X-ray data and images
collected for each particle and another (called MLA
Dataview) to evaluate the compiled results for all
particles and grains in a variety of tables and graphs
or export them to third party software such as
Microsoft Excel.
For the geologist studying sediments or
sedimentary rocks, some of the most useful quantitative data produced by the MLA are for the proportions of minerals in the sample (modal mineralogy);
the amount of void space in the sample (porosity);
the degree of association between pairs of minerals
as measured by the lengths of their shared boundaries (mineral associations); the sizes of particles
and mineral grains in the sample (particle and grain
size distribution); and the shapes of particles in the
sample (particle shape parameters). For modal
mineralogy, wt.% of the mineral is calculated from
area% using an assumed or calculated mineral
density. Volumes of particles and grains may be
calculated from their measured areas using the
diameter of an equivalent area circle or ellipse.
Three shape parameters produced by the
MLA software are particularly relevant for
characterizing detrital minerals: aspect ratio (AR),
shape factor (SF) and angularity (ANG) (e.g.,
Tsikouras et al. 2011). The aspect ratio (AR) is,
AR = LMBR BMBR

A SEDIMENTARY ROCK EXAMPLE

The MLA was used to analyze a sample (10BSG-HL-SS) of a calcite-cemented sandstone from
the Upper Mississippian (Visean) Robinsons River
Formation of the Codroy Group at Crabbes Head,
Newfoundland (Knight 1983), in order to illustrate
some of the capabilities of the method. These
sandstone and associated siltstone units represent
terrestrial clastic sedimentation on river-dominated
flood plains and are interspersed with limestone
units that record regular marine incursions.
The sample was presented to the MLA in
three forms as a standard polished thin section (27
x 46 mm); as a particle mount of the sieved, 63177
m fraction of the crushed sample; and as a
bromoform-concentrated, heavy mineral separate of
the 63177 m fraction. About 5 kg of rock was
crushed and sieved to produce the 63177 m
fraction and about 500 g of that fraction was
processed through bromoform to produce the heavy
mineral concentrate. MLA measurements were
made using an accelerating voltage of 25 kV and
imaging scan speed of 16 sec. The thin section was
measured in GXMAP mode using a beam current of
10 nA and beam diameter of ~125 nm. X-ray
mapping was triggered for a BSE range of 31255;
each X-ray measurement was acquired for 8 msec
with a step size of 10 pixels on a 2 x 2 mm frame
with a resolution of 400 x 400 pixels. Some 88,000
grains were measured. The particle mounts were
measured in XBSE mode using a beam current of 13
nA and beam diameter of ~225 nm. Each X-ray was
acquired for 20 msec. About 23,000 grains were
measured on the mount of the bulk 63177 m
fraction of the crushed sample and 58,000 grains
were measured on the mount of the heavy mineral
concentrate of that fraction.

(3)

where LMBR and BMBR are the length and breadth,

respectively, of the minimum bounding rectangle of
the particle. The aspect ratio provides a twodimensional measure of particle elongation. The
shape factor (SF) is,
SF = P / [2 (A / )]

(4)

where P and A are the surface perimeter and area,

respectively, of the particle. Spherical particles have
a shape factor of 1, though their faces may be
rounded or faceted. Elongated or embayed particles
have shape factors greater than 1. Particles
containing pore spaces or inclusions may have
shape factors less than 1. Finally, angularity (ANG)
is a measure of the irregularity of the perimeter of
the particle (surface roughness) and calculated as,
ANG = (RP REE)2 (REE ) 2

Digital Textural Mapping

Figure 1-6 compares conventional photomicrographs of a petrographic thin section of
sample 10-BSG-HL-SS taken in plane-polarized
light and under crossed polars with the BSE and
false color mineral-keyed images of the same area
produced by the MLA. Visual inspection of the
images indicates that the false color map reproduces
the texture and the mineralogy of the thin section
rather faithfully, albeit with some of the mineral
intergrowths pixelated where they are finer than the
resolution of the mapping used. All of the images

(5)

with RP and REE measured in 1 increments from 1

to 360, where RP is the radius of the particle
measured from its geometric center and REE is the

USE OF THE MINERAL LIBERATION ANALYZER FOR STUDIES OF SEDIMENTS AND SEDIMENTARY ROCKS

Figure 1-6. Images of an area of the polished thin section of calcite-cemented

sandstone 10-BSG-HL-SS made using transmitted light optical microscopy in (A)
plane-polarized light and (B) crossed polars; and using the MLA by (C) BSE
imaging and (D) X-ray mapping with minerals keyed to false colors.
Photomicrographs are taken at 5x (field of view is 2.5 x 1.8 mm).

mapping would be advantageous for studies

requiring examination of large numbers of samples.
Also the MLA technique is able to provide more
detailed maps than that in Fig. 1-6D, showing the
distribution of varieties of minerals in a thin section.
For instance, magnesian and ferroan varieties of
calcite cements could be subdivided on the basis of
X-ray spectra and the distribution of each mapped in
the section, where this information would be useful
for diagenetic interpretations. Accessory minerals
can be identified easily in the digital images
produced by the MLA and targeted for follow-up
in situ chemical or isotopic analyses by laser
ablationinductively coupled plasmamass spectrometry (LAICPMS) or secondary ion mass
spectrometry (SIMS). The ability to analyze
minerals in petrographic context and thus link
composition with rock texture is desirable for many
studies. Linking the digital coordinates for MLA
thin section maps to the stage coordinates of the

indicate that the sample has a grain-dominated

fabric cemented by pervasive intergranular calcite.
The BSE and false color maps clearly show the
absence of porosity in the sample: the few areas
where the MLA detected the glass slide within the
mounted rock slice, which are classified as void
space, appear to be the result of grains being
plucked out of the section during polishing, rather
than original pore space. The BSE and false color
maps also clearly distinguish the quartz and feldspar
grains in the sample, and demonstrate they are
largely monomineralic clasts rather than polymineralic lithic clasts. The locations of accessory
minerals (for clarity, grouped simply as other
minerals in Fig. 1-6D) are easily identified in the
false color map.
While it is true that a careful petrographer
using optical microscopy could determine the same
textural information from the sample as provided by
the MLA, the automated nature of the MLA textural

10

P.J. SYLVESTER

LAICPMS or SIMS can make this task much

easier for the analyst.
Modal Mineralogy
Table 1-1 presents the MLA results for the
modal mineralogy of sandstone 10-BSG-HL-SS in
the thin section and the particle mounts. Quartz,
calcite and K-feldspar are the most abundant
minerals in the sample but the MLA also recognized
several minor minerals, plagioclase, chlorite and
dolomite. A large number of accessory minerals (<1
wt.%) were also found including biotite, muscovite,
hornblende, illite and kaolinite, as well as some
even less abundant heavy minerals (see below).
Based on the bulk, 63177 m size fraction
of the crushed sample, the absolute abundances of
the major minerals are quartz (~49 wt.%), calcite
(~23 wt.%) and K-feldspar (~15 wt.%). However, a
proper estimate of the modal abundances of both
major and minor minerals would require additional
analysis of sieve fractions both finer than 63 m and
coarser than 177 m. The results for each fraction
would be summed according to their weight proportions of the total (5 kg) sample in order to calculate
the best estimate of the modal abundances.
Many more grains were analyzed in the thin
section (~88,000) compared to the bulk, 63177 m
size fraction of the crushed sample (~23,000). This
difference is the result of the more detailed X-ray
mapping carried out by the GXMAP analysis of the
thin section. Nonetheless, a single thin section is
unlikely to provide representative modal abundances for the whole sample given the natural variations present at the kilogram scale in most
sedimentary rocks.
Heavy Mineral Analysis
MLA results for the heavy mineral
concentrate of the bulk, 63177 m size fraction of
the crushed sample demonstrate the expected
enrichment in dense minerals. The MLA data
document enrichment factors (wt.% in concentrate /
wt.% in bulk sample, as given in Table 1-1) of 171
for zircon, 83 for monazite, 52 for chromite, 49 for
allanite, 46 for ilmenite, 34 for magnetite, 19 for
garnet, 15 for rutile and 10 for apatite. BSE and
false color images of the heavy mineral concentrates
(Fig. 1-7) are useful for visual inspection of the
nature of polymineralic intergrowths and choosing
grains for in situ chemical or isotopic analyses. The
images can also be used to troubleshoot problems
with the recovery of unexpectedly large amounts of
light minerals. For example, where minerals such as

Figure 1-7. Images of an area of the 25 mm polished

particle mount of the heavy mineral concentrate of
calcite-cemented sandstone 10-BSG-HL-SS made
using the MLA by (A) BSE imaging and (B) X-ray
mapping with minerals keyed to false colors. Scale
bars shown are 500 m long.

quartz (2.65 g/cc) and calcite (2.71 g/cc) are present

in the concentrates largely as monomineralic grains,
rather than adhering to heavy minerals, there might
be laboratory issues such as dilution of heavy

11

2.20
0.03
0.21
1.10
0.15
0.33
0.37
0.43
0.18
0.50

2.44

0.06

0.20
1.17
0.19
0.49
0.47
0.44
0.32
0.48

Chlorite

Chromite

Cordierite

12
595
12498
951

875200

0.53
3.25
0.11

0.05
0.00
0.03

3.16

0.14

35.78 36.50 302151625

0.17 0.14
1143250
0.01

0.55

0.02

0.06

0.00

0.00

Muscovite

Plagioclase

Pyroxene

Quartz
Rutile

Zircon

Other traces

Non-minerals

Unknown

79125

72

176
1478
88144

40

331

258175

12650

420400

8616

2415

0.13 0.36
3000750
100.00 100.00 827882925

Notes: see next page.

Glass slide
Total

4358225
26902925

0.00

0.00

Monazite

225

19443
1009

13.34 13.55 112157700

0.29 0.15
1270075

K-spar
Magnetite

Ilmenite
Kaolinite

Dolomite
Epidote
Garnet
Hornblende
Illite

1073
3304
860
1678
1930
2018
603
1502

79

7447

1708625
9101725
1266325
2746275
3065150
3554000
1500100
4160500

262825

18212150

39.11 38.96 322555850

Calcite

0.09
0.10
0.66

0.13
0.12
0.73
15972

Grain
Count
626
777175
472
869175
2955
5472725

Wt% Area% Area (m2)

Allanite
Apatite
Biotite

Mineral

Polished Thin Section

Dimensions: 27 x 46-mm, 30 mm thick
MLA Method: GXMAP

100.00

100.00

79988019

12030

22555

Crushed Sample (63-177 m sieve)

Dimensions: 25-mm wide, epoxy round
MLA Method: XBSE
Particle Grain
Wt%
Area% Area (m2)
Count Count
66
79
0.04
0.03
23463
90
108
0.14
0.11
91713
447
584
0.80
0.72
577256
5180
6411
23.48
23.44 18748744
1367
2033
4.22
3.81
3047744
13
13
0.16
0.09
73350
47
58
0.07
0.08
61250
233
282
0.39
0.37
295844
39
40
0.05
0.04
29431
195
231
0.39
0.26
205481
137
156
0.15
0.12
95169
216
255
0.56
0.55
437494
133
164
0.70
0.39
315038
35
37
0.02
0.02
17088
2851
3459
15.18
15.46 12365094
260
373
0.45
0.23
187831
2
2
0.00
0.00
475
261
331
0.57
0.55
439144
1030
1203
3.54
3.64
2913956
48
52
0.06
0.04
33588
5907
6227
48.76
49.80 39830175
217
301
0.21
0.15
122950
22
22
0.02
0.01
10419
12
12
0.03
0.02
15281
26
26
0.00
0.00
294
6
6
0.00
0.00
338
85
90
0.02
0.06
49413
100.00

100.00

108798032

20122

58439

Heavy-Mineral Concentrate (63-177 m sieve)

Dimensions: 25-mm wide, epoxy round
MLA Method: XBSE
Particle Grain
Wt%
Area% Area (m 2)
Count Count
1115
1684
2.01
2.09
2273295
523
639
1.30
1.60
1742109
1703
3651
1.99
2.63
2857680
4997
6808
8.38
12.22
13297818
3180
6582
5.55
7.31
7955095
1509
1574
8.48
6.99
7606358
135
180
0.17
0.25
270397
495
675
0.30
0.40
438893
57
61
0.02
0.02
25486
1805
2062
7.45
7.05
7668332
315
377
0.16
0.19
203804
409
624
0.30
0.43
472900
6397
8823
31.87
26.24
28548319
141
176
0.05
0.07
75922
1732
2530
2.15
3.16
3437489
4884
9776
15.36
11.88
12920326
41
48
0.09
0.07
78306
342
543
0.31
0.43
466811
813
990
0.70
1.05
1146787
249
542
0.20
0.21
224994
3242
4196
5.99
8.93
9713005
2232
4421
3.13
3.27
3559194
795
818
3.87
3.25
3538187
206
245
0.17
0.18
193216
61
61
0.00
0.00
281
226
278
0.00
0.06
60547
73
75
0.01
0.02
22484

TABLE 1-1: MODAL MINERALOGY OF SANDSTONE 10-BSG-HL-SS DETERMINED BY MLA ON THIN SECTION AND PARTICLE MOUNTS

USE OF THE MINERAL LIBERATION ANALYZER FOR STUDIES OF SEDIMENTS AND SEDIMENTARY ROCKS

P.J. SYLVESTER

Notes for Table 1-1.

Number of particles not given for thin section because the MLA effectively treats each frame measured as a
particle in this case
Total number of particles for particle mounts is less than the sum of the column because most particles contain
more than one mineral
A small amount of calcite includes minor amounts of fine-grained intergrown feldspar and pyrite
Chlorite is dominantly Fe-rich and a minor amount contains minor intergrown mica
Dolomite includes ankerite and minor intergrown silicate
Epidote is clinozoisite and piemontite
Garnet is mainly almandine, but also includes subordinate grossular and andradite
Hornblende also includes actinolite, some of which contains fine-grained intergrown chlorite
K-spar includes some fine-grained intergrown quartz and more rarely, pyrite
Magnetite includes titanomagnetite and minor hercynite
Plagioclase is dominantly albite
Pyroxene includes diopside and ferrosilite
Rutile is in part altered and minor amounts are intergrown with fine-grained quartz
Other trace minerals (each <0.05 wt.%) are baddeleyite, barite, native copper, corundum, gehlenite, goyazite,
halite, kyanite, pyrrhotite, rhabdophane, serpentine, thorite, titanite, xenotime-(Y)
Non-minerals are the sample holder, or areas with low or no X-ray counts, representing polishing artifacts or
grain edge effects
Unknowns are unidentified minerals
Void space is where the glass slide was detected within the dimensions of the rock slice in the thin section or
epoxy was detected within particles in the round mounts

have areas of 30009000 m2, aspect ratios of

~12, shape factors of ~1.11.3, and angularity
values of ~240. A subordinate population of
liberated zircon grains is also present however: it
forms smaller, more elongate and angular grains
with areas of 400 2000 m2, aspect ratios of ~25,
shape factors of ~1.31.8, and angularity values of
~40600. The morphology data for the zircon are of
course limited by the sieve size fraction (63177
m) processed for the concentrate but there is a
suggestion that there are zircon grains in the sample
with two broadly different origins. High resolution
BSE and cathodoluminescence imaging would be
able to show whether the smaller grains are simply
broken fragments of the larger grains. If they are
not, in situ chemical and isotopic analyses of
representative grains from each population could be
used to explore the nature and origin of their
differences in more detail.

liquids by repeated washing with acetone (0.79

g/ml). The quantitative modal abundance data
provided by the MLA on the heavy mineral
proportions may be used to calculate mineral indices
(e.g., chrome spinel/zircon and garnet/zircon) used
for evaluations of provenance (Morton 2012) or
diagenesis (Pe-Piper & Piper 2012).
Zircon Grain Morphology
As noted above, the MLA software has the
capability of determining the size distribution of
both particles and mineral grains in an analyzed
sample. In addition, the software calculates a variety
of shape parameters for particles: if shapes of grains
of a particular mineral species are of interest, the
parameters may be calculated for monomineralic
particles of the mineral of interest alone. As an
example from sandstone 10-BSG-HL-SS, morphologic properties of zircon in the heavy mineral
concentrate are shown in Fig. 1-8. Detrital zircon in
sediments and clastic sedimentary rocks is of
considerable interest because the mineral preserves
a record of UPb age and Hf-isotope composition
that is useful for studies of provenance, stratigraphic
correlation and crustal evolution (see Koler 2012).
A total of 818 grains of zircon were identified
in 795 particles by the MLA analysis (Table 1-1)
and 601 of those grains were completely liberated,
forming discrete monomineralic particles. The
majority of liberated zircon grains in the concentrate

FUTURE PROSPECTS
Application of the MLA to sedimentary and
surficial geology is in its infancy but the method
holds considerable promise for providing quantitative data relevant to depositional and diagenetic
textures and mineralogy; porosity and permeability;
sand provenance; stratigraphic correlation; lithotyping of well cuttings; till and sediment
prospecting; sedimentary ore petrology; and
environmental mineralogy. From an analytical

13

USE OF THE MINERAL LIBERATION ANALYZER FOR STUDIES OF SEDIMENTS AND SEDIMENTARY ROCKS

Figure 1-8. Morphology data for discrete (completely liberated) zircon grains (n=601) measured in the 25 mm polished
particle mount of the heavy mineral concentrate of calcite-cemented sandstone 10-BSG-HL-SS. Size of zircon grains
(expressed as area) plotted as (A) a histogram of the numbers of grains (binned in increments of 2000 m2), and against (B)
aspect ratio, (C) shape factor and (D) angularity of the grains.

standpoint, several outstanding issues remain for

the MLA method. Techniques for the discrimination
of certain difficult mineral pairs need
additional attention, as recently has been the case
for hematite and magnetite. These minerals are
simple iron oxides that differ in Fe content by
only 2.5 wt.%, making them nearly impossible to
distinguish on the basis of EDX analysis, but
also have very similar greyscale values in BSE,
which are not easily distinguished (Shaffer 2009,
Figueroa et al. 2011). Also, MLA methods need to
be tested and verified more extensively with
well-characterized reference materials to better
define limits on accuracy and precision of
measurements. Procedures for data handling and
reporting should become more normalized so that
result from different laboratories can be compared
more directly. With these efforts, and through
dedicated training of university students and
professionals in MLA methods, it is likely that
the MLA and related techniques such as
QEMSCAN and CCSEM will assume increasing

prominence in geological laboratories throughout

this decade.
ACKNOWLEDGEMENTS
I have benefited greatly from the expertise
and advice of Michael Shaffer who has managed
and developed the MLA laboratory at Memorial in
an efficient and innovative manner since 2004.
Michael has also made important contributions to
development of the MLA technology in general, in
particular on the integration of silicon drift detectors
with the instrument; measurement procedures for
overcoming problematic mineral discriminations
such as between hematite and magnetite; and
improved laboratory protocols for producing
representative particle mounts. Lauren Flynn drafted
the figures in the chapter and carried out the MLA
data reduction for the example sedimentary rock.
Michael Shaffer and Kate Souders provided helpful
comments on the manuscript.

14

P.J. SYLVESTER

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16