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5.1Introduction
Improved characterization of lower-grade iron ores is becoming more critical owing
to the depletion of world high-grade iron ore reserves. The mineralogy and gangue
minerals of the lower-grade iron ores are found to affect the quality of pretreated ag-
glomerates of fine ore (sinters and pellets), which are making up a growing proportion
of blast-furnace feedstock (currently ~70 % in East Asia).
The understanding of lower-grade iron ore mineralogy and the subsequent char-
acterization of lower-grade iron ore are therefore becoming increasingly important
to the efficient processing of the ores and the optimization of downstream smelting
processes.
Using scanning electron microscope (SEM)-based technologies to characterize and
quantitatively analyze iron ores and iron ore mineralogy dates back to the invention
of the technology in the late 1950s to the early 1960s. The emphasis shifted from the
chemical analysis of penalty elements on microprobe systems to quantitative mineral-
ogy on automated mineralogical systems (auto-SEMs) only relatively recently (early
1990s). However, auto-SEMs consistently struggled to differentiate between the most
common iron oxides present within iron ore, those being magnetite (Fe3O4) and he-
matite (Fe2O3), since auto-SEMs traditionally used energy-dispersive spectroscopic
(EDS) technology for Fe quantification and furthermore ran at low X-ray counts.
Assay reconciliation, by comparing the amount of Fe measured from chemical analy-
ses against the calculated amount of Fe in a sample based on its mineralogy, was thus
essential for these systems, in gaining some kind of grasp on the amount of hematite/
magnetite in an ore body up until about 2008 and often required further X-ray diffrac-
tion (XRD) analysis for confirmation, which with the advent of Rietveld analysis has
become more quantitative in recent years.
Improved beam, system, and vacuum stabilities and in some instances stretched
brightness/contrast signals resulted in better, more consistent backscattered electron
(BSE) imaging, which allowed for better magnetite/hematite discrimination. With the
arrival of an appropriate level of hematite/magnetite distinction came the ability to use
the input of theoretical densities to predict the performance of various mechanisms of
density separation, mostly sink-float or washability analysis (B. Ntsoelengoe, 2011,
personal communication). Also, with an appreciation of the different chemistries dis-
tinguishing acicular SFCAs from columnar/tabular SFCAs, the analysis of iron ore sin-
ters in these systems was relooked at from about 2010 (Toneti and Dippenaar, 2011).
With this came the realization that auto-SEMs, in one form or another, could be used
for mineralogical quantification through the project flow cycle, from exploration
(where bulk ore mineralogy was most important), to mining (recently geometallurgi-
cal modeling), to processing (concentrator/mining products), to utilization (sinter and
pellets; Table5.1). Auto-SEMs even found application in the characterization of iron
ore mine overburden, consisting mostly of pedocrete (Toneti, 2012). This proved
vital since it had a direct bearing on the calculations of the amount of overburden
occurring over the deposit, which in turn related directly to the cost of the overburden
removal (usually calculated on mass/density and not volume). Of specific note was
the occurrence of swelling clays (smectite) that had a direct bearing on the volume of
overburden encountered, though XRD is still a better technique for clay mineral spe-
ciation since many clay minerals have similar chemistry but different lattice structures.
l = h /p
a
Silicoferrite of calcium and aluminum, a product of sintering low-grade fine iron ore to create a feed for blast furnaces. For more information, see Toneti and Dippenaar (2011).
164 Iron Ore
Primary
Backscattered electron beam
electrons
Characteristic
X-rays
Secondary Cathodoluminescence
electrons
Transmitted
electrons
core, since most iron ore is sedimentary in origin, great care must be taken to ensure
that the area for cutting is in profile across bedding planes to maximize the discrimi-
nation of any textural features.
(SIP files in the case of QEMSCAN, standard files in the case of MLA, and recipes
in the case of Mineralogic (R)) seldom account for both methods of mineral identifi-
cation due to historical paradigms. All these instrument paradigms have much to do
with the chamber/detector geometry and the traditional SEM setup of the developing
companies. Off-line data mining (which includes the off-line replaying or reanalysis
of datasets after mineral identification rules have been changed) and graph plotting are
possible with all the systems.
Differences in the values of quantities between auto-SEMs and other technologies
do occur, since the auto-SEM classification of minerals is based mostly on chemical
composition while traditional classification through XRD is based on crystal structure.
Also, whereas point-counting results (from light microscopes) are typically presented
in terms of area percent and XRD results are typically presented in terms of weight
percent, auto-SEM results are typically presented in terms of both area and weight
percent (calculated based on input density values since auto-SEMs cannot measure
density directly).
Since most auto-SEMs prefer flat surfaces for measurement (like light microscopes)
to avoid X-ray shadowing and the proper application of ZAF correction factors in the
EDS analysis, cognizance should be made of the fact that the morphological interpre-
tations of sections have limited value as evidenced in Figure5.2. Light microscopes
suffer from the same limitation. Historically, this is what has limited SFCA characteri-
zation on auto-SEM systems (though the same argument/limitation should be used for
light microscopes that have traditionally studied sinters).
3
1
average atomic numbers. Problem minerals therefore encountered in analysis may in-
clude hematite and magnetite since they share similar chemistries and similar average
atomic numbers. Goethite may also be problematic in identification, though it usually
contains sufficient impurities to help differentiate it from hematite, in auto-SEM sys-
tems. It is therefore important to note that auto-SEM distinctions between magnetite
and hematite are dependent on a number of factors, specifically the surface characteris-
tics of the iron oxides being measured (scratching, plucking, dipping beneath mounting
media, porosity, carbon coating thickness, etc.) and the degree of ionic substitution
being encountered in the iron oxides (in particular Mg, Ca, Al, and Mn).
Iron oxide discrimination on auto-SEM systems can furthermore be influenced by
BSE stabilizers (also known as BSE amplifiers) on certain systems, gun alignment
(essentially whether the electron beam is coming down the column unhindered with
no shadowing of the beam), and magnification field sizes. Furthermore, stage height
(working distance) focus primarily determines grayscale, while beam focus has an
effect on BSE grayscale averaging (and the image focus itself). Appropriate third point
BSE calibration standards and increased beam dwell times (i.e., giving the electron
beam more time on a specific point to make an identification) improve discrimina-
tion. Image analysis and processing can do away with certain artifacts of analysis.
Auto-SEM instruments make use of their own paradigms to reduce or eliminate some
of the abovementioned problems, though no single instrument eliminates all of them.
Figure5.3 presents images of an electron microprobe hematite standard measured in a
QEMSCAN system with different measurement parameters. The following sections look
more closely at the instrument types and varieties. Table5.2 highlights their differences.
5.2.3.4QEMSCAN
QEMSCANs were previously produced by Intellection on Carl Zeiss EVO platforms
(Pirrie etal., 2004; Gottlieb et al., 2000; Sutherland and Gottlieb, 1991). Currently,
QEMSCANs use FEI Quanta and field emission gun (FEG) platforms for their op-
eration. QEMSCAN instrumentation uses computer grayscale BSE imaging in con-
junction with a custom-designed X-ray spectral window database to identify phases
of interest. The QEMSCAN technique tends to produce X-ray maps, whereby EDS
X-ray spectra are collected at predefined beam-stepping intervals, at lower magnifi-
cations/higher field sizes (because of historically poor imaging). Because of its em-
phasis on X-ray collection, it is a preferred method for characterizing solid solutions
(where BSE grayscale is not amenable to species differentiation), finely intergrown,
chemically complex textures, and silicates, since EDS analyses are taken every couple
of microns (typically between 1 and 20 m). In recent years, QEMSCAN has focused
on collecting X-ray elemental concentration data (rather than data on X-ray spectral
windows) although QEMSCAN systems still favor superior X-ray collection.
5.2.3.5MLA
Previously manufactured by JKTech (the technology transfer company for the
Sustainable Minerals Institute housed in the Julius Kruttschnitt Mineral Research
Centre of the University of Queensland, Australia) on FEI Quanta platforms, MLAs
168 Iron Ore
(a) (b)
(c) (d)
(e) (f)
are now manufactured wholesale by FEI (Figueroa etal., 2011). MLA instrumen-
tation uses a best-fit model to compare collected EDS X-ray spectra with a spectral
library. The MLA technique tends to produce X-ray centroid measurements, whereby
single EDS X-ray spectra are collected for common BSE grayscale levels, at higher
magnifications/lower field sizes and is thus a preferred technique for small grain sizes
and high-resolution imaging. The MLA favors superior imaging over EDS collection.
In recent years, MLA data have been made compatible with QEMSCAN iDiscover/
iExplorer software, since it is more versatile for data interrogation and processing. A
novel feature of the MLA system is the ability to produce initial spectral collection
surveys where type spectra are collected for common BSE grayscales. The approach
Quantitative analysis of iron ore using SEM-based technologies169
of the MLA system typically means that most systems use single-spectral libraries and
are also more beginner/user friendly than QEMSCANs.
5.2.3.6Mineralogic (R)
The Mineralogic (R) (and TIMA, discussed below) auto-SEMs are the newest au-
tomated mineral analyzers on the market. The Mineralogic (R) system is manufac-
tured by Carl Zeiss and favors image processing and image analysis that occurs during
the automeasurement to discriminate between the sample and mounting media (Hill,
2014). Unlike the QEMSCAN and MLA systems, analysis times are requested and
not analysis counts. The analysis involves a parallel two-stream approach where im-
age processing/image analysis forms one stream (and is in the control of the operator
unlike traditional auto-SEM technologies) and energy-dispersive X-ray analysis forms
a second stream (similar to more traditional technologies). The X-ray analysis and
image analysis can then be recombined to form a higher-order classification. This
may allow for mineral variety classifications in the future whereby, for instance, a
hematite spectral assignation occurring in a mineral grain of a specific shape might be
called specularite, theoretically. The Mineralogic (R) system also allows for a degree
of correlative microscopy whereby it is possible to georeference or correlate images
from different technologies (light microscopy, cathodoluminescence, secondary elec-
tron images, etc.) with those seen in the auto-SEM to facilitate mineral identification
(especially magnetite/hematite distinction).
Mixed spectral resolution often referred to as boundary phase processing (getting rid of
or reclassifying mixed spectra occurring at boundaries between mineral grains of different
composition).
Granulating (through erosion/dilation algorithms; typically used to extract grains of eco-
nomic interest for further processing).
Field stitching (used for large particulates/slabs/cores that take up more than a single field of
view during measurement).
5.3.1Textural analysis
The state of the art for the latest auto-SEM technologies, in terms of textural analysis,
is mostly visual, although iDiscover (QEMSCAN software) does allow for catego-
rizing particles or grains on x- and y-axes creating what are termed image grids. The
properties that can be used to create those categories (things like shape factor) are,
however, somewhat limited. The MLA and Mineralogic (R) systems have far more
categories for interrogating shape. However, they lack the flexibility of being able to
create image grids. Textural images of conglomerate, measured with a QEMSCAN
system, are presented in Figure5.6.
5.3.2Mineral abundance
Table5.3 presents a typical example of how mineral abundance is presented in
auto-SEM analyses. Usually these data are presented in terms of mass percent. All
auto-SEM systems allow for first-order mineral identification (the SIP files, standard
files, and mineral identification recipes mentioned above) and first-order groupings
where mineral densities (and other mineral qualities) are assigned and second-order
groupings are simplified to make data interpretation easier and more relevant. So, in
terms of work flow, a QEMSCAN system may identify a zircon and a metamict
zircon from its SIP files, group these together in a primary mineral list (first-order
grouping), and further group these along with other minerals in an others grouping
(secondary mineral list) if there is not enough zircon to warrant specifying it in a min-
eral abundance table.
5.3.3Magnetite/hematite distinction
The analysis of iron oxides in automated mineralogy is primarily based on grayscale
values that are directly proportional to an average atomic number. It can thus occur
that, with atomic substitution (for instance, Mg or Ca for Fe), the average atomic num-
ber of magnetite can be lowered, resulting in a lower grayscale value, with a resultant
overestimation of hematite and an underestimation of magnetite. A pure hematite or
magnetite standard can be used as a third point calibration for both the QEMSCAN
and MLA systems although QEMSCAN typically uses copper as a third standard while
MLA uses chalcopyrite (Figueroa et al., 2011). Using a synthetically or artificially pure
standard might not negate these misidentifications always, since in naturally occur-
ring hematite, Fe can be substituted with Al, for instance, and in naturally occurring
172
Table5.3 A typical example of the bulk mineral abundance for conglomeratic iron ores
Chlorite/
Id Hematite Quartz Feldspar Mica clay Phosphates Pyrite Others Total
C1 40.9 57.0 0.0 0.2 1.1 0.4 0.0 0.3 100.0
C2 55.8 0.0 0.0 40.8 2.1 0.3 0.0 0.9 100.0
C3 74.1 20.2 0.1 1.5 2.3 1.4 0.0 0.4 100.0
C4 97.0 0.0 0.0 1.0 1.5 0.2 0.0 0.4 100.0
C5 33.0 0.0 0.0 0.2 63.2 0.1 0.0 3.4 100.0
C6 94.0 0.0 0.0 0.0 5.4 0.1 0.0 0.5 100.0
C7 78.5 0.0 0.0 15.9 1.5 0.3 0.0 3.8 100.0
C8 60.2 14.8 0.0 1.7 22.5 0.3 0.0 0.4 100.0
Iron Ore
Quantitative analysis of iron ore using SEM-based technologies173
magnetite, Fe can be substituted with Ca and Mg. Using a properly characterized standard
from a specific ore deposit may correct for this, bearing in mind that grayscales can
still be affected by mineralmineral or mineralbackground edge effects, particle relief
(minimized with appropriate polishing techniques), and porosity.
5.3.4Lithotyping/microlithotyping
The use of filters or categorizers and especially the creation of image grids (based on
whether particles are intuitively of a certain type) in iDiscover software allow for the
creation of rules that can separate particles into lithotypes, or rather microlithotypes.
Mineralogic (R) also allows for the very basic creation of expressions, usually the
addition of the quantity of two different minerals in an analysis, which are used to
classify particles during the measurement into defined microlithotypes. Since there is
no consistency between how QEMSCAN, MLA, and Mineralogic (R) (or any other of
the auto-SEMs) create these expressions, none of them can be moderated into standard
types that would correspond with geologic definitions of lithotypes. The software of
the various auto-SEMs also allows for very basic plotting of properties on ternary dia-
grams, with the three axes being limited to the particle properties that can be extracted
from the relevant software suites.
5.3.5Grain size
Since beam-stepping intervals (in the case of X-ray mapping) or pixel sizes (in the case
of X-ray centroiding) are always known and since this information can be counted for
contiguous classified pixels in mineral grains, grain size can be readily calculated
for mineral grains. Most particle/grain sizes are usually recalculated and reported as
equivalent circular diameter (ECD) values though this not necessarily always correct or
meaningful especially in the case of hematite bands in a banded iron formation (BIF).
An extracted hematite band converted to an ECD is meaningless. What must also
always be remembered is that the grain size calculated is very much dependent on the
magnification calibration of the individual instrument (and this is usually dependent
on the skill of the instrument service engineer).
authors, etc., since different processing mechanisms are amenable to different mineral
properties and ore textures. Thus, a gravity or density separation procedure would ne-
cessitate liberation characterization based on the area percent of a mineral of interest
in a particle, whereas a leaching concentration procedure would necessitate liberation
characterization based on the free surface area percent (exposure on a particle surface)
of a mineral of interest in a particle. This latter, free surface area percent liberation
is called, by some authors, locking although the term locking is also applied to
minerals of interest sorted according to their association in an image grid with other
minerals, once all liberated mineral grains have been removed from an analysis. Here,
association is typically represented as the occurrence of binary particles where if a
particle constitutes more than 80% hematite and quartz, for instance, then it is classi-
fied as a hematite-quartz binary particle. These associations are subsequently quan-
tified. To avoid confusion, the proper use of the term association, it is felt, should be
restricted to the property of adjacency, where two minerals are associated, if they
are adjacent to one another. The number of occurrences of adjacency (as long as it is
specified as left-right pixel occurrences, top-down pixel occurrences, or both) can be
counted and converted into a percentage, and this would quantify an association be-
tween two minerals of interest.
Liberation is typically divided into categories based on 10% subdivisions of the
area percent occurrence of a mineral of interest (for instance, hematite) within a par-
ticle. Thus, particles are separated into 010%, 1020%, 2030%, etc., categories and
plotted on 3D charts with size fractions, liberation categories, and their weighting
(mass percent) being plotted on three axes, based firstly on unnormalized discrete
values (values that add up to the absolute amount of hematite in the total sample) to
normalized head (absolute) values (hematite is normalized to 100% for the total
sample) to normalized fraction (relative) values (hematite is normalized to 100%
per size fraction). These normalizations allow for the cumulative plotting of liber-
ation values on common graphs and allow for the direct comparison of liberation
between different samples, size fractions, etc. These liberation categories are usually
further simplified by grouping them in 20% categories. Thus, particles in the 020%
class are usually called locked, 2040% are lower-grade middlings, 4060% are
medium-grade middlings, 6080% are high-grade middlings, and 80100% are
liberated. Some workers suggest also using 0% (gangue) and 100% (fully lib-
erated) categories though since we are dealing with the 2D analysis of surfaces in
auto-SEMs, these categories are strictly speaking invalid since we cannot make
assumptions about the occurrence of hematite below (and eroded above) the sur-
face that has been analyzed.
As can be seen, the liberation characterization of minerals of interest in auto-SEM
systems is hardly trivial. Though with the direct input of mineral characteristics (such
as electrostatic affinity, floatability, and magnetic susceptibility) into auto-SEM an-
alytical programs and the understanding of particle characteristics (area percent liber-
ation vs. surface area percent liberation) that make minerals amenable to processing,
the reliance on liberation (as is currently conventionally used) may be reduced in the
future, with more of a direct reliance on the calculated processability of an ore.
Quantitative analysis of iron ore using SEM-based technologies175
Figure5.4 Image of originally measured slab and subsequent granulation of dark gray/black
hematite clasts with erosion and dilation operations having subsequently been applied.
White represents (vugular) macroporosity.
176 Iron Ore
3000.0 m
3000.0 m
Figure5.5 Hematite granulation applied to BIF samples. Note the interconnectivity across
hematite bands, which suggest the fracturing and remobilization of hematite.
80
70
60
Mass % hematite
50
40
30
20
10
0
>0 >250 >500 >750 >1000 >1250 >1500 >1750
Clast size (mm)
100
90
80
Cumulative mass % hematite
70
60
50
40
30
20
10
0
>0 >250 >500 >750 >1000 >1250 >1500 >1750 >2000 >2250 >2500 >2750 >3000 >3250 >3500
Clast size (mm)
C1 C2 C3 C4 C5 C6 C7 C8
80
70
60
Mass % hematlte
50
40
30
20
10
0
>20 >40 >60 >80 >100 >120 >140 >160 >180 >200 >220 >240 >260 >280 >300 >320
Band width (mm)
100
90
80
70
60
Mass %
50
40
30
20
10
0
500
1500
2500
3500
4500
5500
6500
7500
8500
9500
10,500
11,500
12,500
13,500
14,500
15,500
16,500
17,500
18,500
19,500
20,500
21,500
22,500
23,500
24,500
25,500
26,500
27,500
28,500
29,500
30,500
31,500
32,500
33,500
34,500
Stepping interval
Figure5.10 Demonstration of the subjectivity of defining band widths for sample B7 with the
occurrence of quartz microbands. Hematite composition is black while quartz is light gray.
system. Point-counting and XRD results provided for quantification baselines, bearing
in mind the inherent pitfalls that could be (and in some cases indeed were) found in
these types of abundance analyses. Table5.6 presents a basic comparison of mineral
distinction between QEMSCAN and point-counting techniques. Table5.7 presents
modal results of QEMSCAN against point-counting. Both these tables put in con-
text difficulties that can be encountered in both techniques when it comes to mineral
identification, for instance, Loo (1998) suggested that it is virtually impossible to dif-
ferentiate magnesioferrite from magnetite under optical microscope point-counting
conditions, whereas a magnesium X-ray signature is essential for QEMSCAN iden-
tification and is readily measured. Table5.8 presents a comparison of QEMSCAN
results with the Topas and Autoquan results (both XRD methods of measurement). In
Table5.8, an increase in magnetite is seen with an increase in magnesium (consistent
with Hsieh and Whiteman, 1993 and Oluwadare, 2007), with the increase being more
pronounced in the QEMSCAN results (as evidenced by the magnetite to hematite
ratio). High aluminum appears to promote SFCA formation as seen by the high SFCA
to calcium ferrite ratio (consistent with Oluwadare, 2007), with the results once again
being more prominent for the QEMSCAN analysis. The QEMSCAN results also sug-
gested the preferential formation or stabilization of hematite with an increase in alu-
minum (consistent with Oluwadare, 2007). Toneti and Dippenaar (2011) discussed
extensively possible reasons for the differences encountered in the SFCA modal
abundances between the various technologies but pointed to vague and inconsistent
180 Iron Ore
Hematite
Quartz
0 mm 5 mm 25 mm
Figure5.11 An example of a BIF measured within a QEMSCAN system. White represents
(vugular) macroporosity.
All auto-SEMs allow for the input of standard mineral density values into their
analytic programs. It is therefore possible to calculate the average density of any
given measured particle by adding together the area fractions of minerals occurring
in a particle multiplied by their appropriate inputted densities. It is then possible to
place these minerals into density classes or categories and to plot a mass percentage
histogram. This is enough to gauge a rough idea of ideal heavy liquid separation
parameters for dense liquid separation, though by itself gives no idea of grade. If the
increasing cumulative percentage of iron is plotted along the same axes, along with
the decreasing cumulative percentage of any major gangue element (usually silicon),
the grade (and amount of deleterious element concentration) of a given concentrate
can be predicted if dense media separation is carried out at a specified dense liquid
cutoff. Conversely, if a specific grade of concentrate is required, it can be found on
the graph and the appropriate density of liquid needed can be selected (Richardson
and Morrison, 2003).
Quantitative analysis of iron ore using SEM-based technologies183
Table5.7 Comparison of QEMSCAN (QS) results against point-counting (PC) results (area %)
Sample 1 Sample 2 Sample 3 Sample 4
Mineral QS PC QS PC QS PC QS PC
Magnetite 6.3 12.8 3.2 7.8 9.4 7.0 5.8 8.1
Magnesioferrite 0.8 16.7 0.9 22.3 0.8 21.3 0.5 18.1
Calciomagnetite 13.0 0.0 11.5 0.0 12.5 0.0 12.4 0.0
Hematite 27.6 21.0 32.1 25.9 24.9 20.5 30.3 21.2
Calcium ferrite 30.4 11.3 29.3 6.4 30.7 6.2 33.0 14.9
SFCAa 18.4 35.2 17.4 32.7 16.5 40.8 14.8 35.9
Calcium silicates 0.4 0.0 1.0 0.0 0.3 0.0 0.1 0.0
Glass 3.1 3.0 4.6 4.9 4.9 4.2 3.1 1.8
Total 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0
a
Silicoferrite of calcium and aluminum.
184
Table5.8 Comparison of QEMSCAN (QS) results against XRD Topas and Autoquan (AQ) (weight %)
with additional chemistry
Name Sample 8 Sample 9 Sample 10
Aluminum 1.0 1.0 1.1
Magnesium 0.7 1.4 1.4
Mineral QS TP AQ QS TP AQ QS TP AQ
Magnetite 35.3 35.5 39.3 48.0 40.7 42.1 37.2 50.6 51.7
Hematite 22.2 34.7 33.3 11.2 24.9 25.2 25.5 24.3 24.6
Calcium ferrite 15.5 9.4 7.0 14.2 10.5 11.7 9.5 7.9 6.0
SFCA 20.1 12.6 12.8 19.1 12.8 11.5 18.5 10.0 11.0
Ca silicates/glass/ 6.9 7.8 7.6 7.5 11.1 9.5 9.3 7.2 6.7
others
Total 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0
SFCA/CFa 1.3 1.3 1.8 1.3 1.2 1.0 1.9 1.3 1.8
Mag/Hemb 1.6 1.0 1.2 4.3 1.6 1.7 1.5 2.1 2.1
Iron Ore
Quantitative analysis of iron ore using SEM-based technologies185
5.5Summary
The relative strengths and weaknesses of automated SEM-based technologies for the
characterization of iron ore samples, compared with manual techniques, are summa-
rized below.
5.5.1Advantages (strengths)
While most auto-SEMs are not entirely operator-independent, they, to a large extent,
allow for the automatic collection of data once a measurement run has been initiated.
They are accurate once they have been taught what they need to know (though
this usually resides within the intellectual property of the operator or purchaser,
this does allow for a certain competitive advantage to be gained from purchasing an
auto-SEM and training it to do very specific measurements). Auto-SEMs are quick
with typical point analyses occurring in the region of milliseconds and measurement
runs per s ample block typically being resolved within 14h. There is no doubt that
these techniques are repeatable. Their consistency between testing runs is unparal-
leled. They remove the tedium of manual analyses often associated with microprobes
and more complicated instrumentation. While being expensive (in the order of 0.61.2
million US$), they are by no means the most expensive of analytic equipment and can
be cost-efficient since they can be run automatically after business hours and during
weekends. The fact that they can be left to run by themselves also means that they are
time-efficient in that operating mineralogists and metallurgists can be preoccupied
with other duties while their instruments are running.
The statistically valid data that are generated by these instruments run into the thou-
sands to millions of analysis points per measurement (approximately 10,000 times
greater number of analysis points than those obtained by point-counting) and most
can record and monitor variation during measurement to allow for project manage-
ment and quality control. The generation of these statistics means that work previously
considered impractical is now possible and that one is more likely to simply measure
for the sake of empirical experiment. Any single particle, collected and measured, can
be treated as a single particle or as part of a set of particles. As a single particle, its
properties are not hidden in a plethora of tables, modal results, and bulk data. These
auto-SEMs can, in a sense, be both holistic and atomistic.
5.5.2Disadvantages (weaknesses)
As has already been mentioned, for all SEM-based systems, potential difficulties in
analysis occur when phases of similar chemistry have similar average atomic numbers
(i.e., similar BSE intensities). These difficulties are minimized with appropriate stan-
dards, best practice methodologies including the stretching of contrast and the use of
multiple measures in combination (BSE, X-ray information, elemental ratios, etc.) to
increase confidence in analyses.
Further, there are a number of difficulties associated with automated im-
age analysis including the delineation of hematite clasts against hematite matrix
186 Iron Ore
Far be it from the scope of this chapter to elaborate on the possible causes of these
errors, for each of the above, the reader will briefly be made aware of where errors can
creep into an analysis by point form in Table5.5 (for more information, consult the
references at the end of this chapter and the author). Measurement errors are usually
less significant than sample preparation errors because, to a certain extent, they can
be compensated for in the mineral identification rule sets and can also, once again to
a certain extent, be corrected for in data processing by experienced operators. So, for
instance, boundary or edge effects can be accommodated for in mineral identification
rule sets by accounting for the presence of carbon (among other elements) from epoxy
resin and graphite fillers. Also, any unidentified (mixed spectral or boundary) phases
can be resolved into legitimate mineral entries by various data-processing strategies
(Toneti, 2014). More grave errors usually creep in with sample preparation (relief
artifacts, bubbles, plucking, smearing, scratching, etc.) and inexperienced auto-SEM
operators attempting to compensate too much for instrument physics (for instance, by
increasing mineral identification windows to limits that will catch multiple different
minerals within a single entry).
5.6Future trends
Doubtless, auto-SEMs will get faster, smarter, be more accurate, and be more au-
tomated in the future, the speculation of which lies in the how. Faster no doubt
lies in the improved performance of EDX spectrometers. In a single generation, liquid
nitrogen detectors were eclipsed by SDDs (silicon drift detectors), which were 4 times
quicker and doubtless will get faster in the future in terms of analysis speeds.
Quantitative analysis of iron ore using SEM-based technologies187
In terms of accuracy, detector quality is sure to improve and may in the future
approach the same level of elemental differentiability as WDS detectors though this
will probably require the writing of some very smart rules or code that operate in the
background of auto-SEM runs.
Smarter auto-SEMs will no doubt entail an improved query language especially
for textural evaluation, so that an operator mineralogist can bring up or return any
particles of interest that obey or observe any quality that has been measured directly
or calculated indirectly by inference. Many auto-SEM software programmers have
maintained (and doubtless will always maintain) that the data are all there It's just
a question of bringing it out. Forays into this area have already been made with most
auto-SEMs being able to at least accept additional data characteristics of minerals
other than the ubiquitous density (values such as flotation indices). Smarter query
languages or even smarter measurement variables may in the future allow for the dis-
tinction of mineral varieties based on their morphologies or textures. So, for instance,
specularitic varieties of hematite may be distinguished from martitic varieties of he-
matite based on shape factor (compactness, aspect ratios, etc.) or even their associ-
ation with pores (porosity). A smarter (or at least more integrative) approach in the
future may allow for the possible incorporation of cathodoluminescence (or any other
analysis method resulting in a multispectral approach) as a tool in grain segmenta-
tion or even further identification of minerals in iron ores (and other commodities).
Correlative microscopy that would combine SEM and optical approaches (and even
XRM) to overcome issues associated with the differentiation of phases with similar
chemistry and BSE values (magnetite and hematite) can most definitely add value to
iron ore quantification. This approach would not be far removed from the integrative
geographic information system (GIS) approach in common use for macro (large-
scale) geographic mapping.
More automated one-button approaches have already been developed by some
of the auto-SEM companies though great care and caution should be exercised with
these instruments to ensure valid datasets. As always quicker, less-intensive measure-
ment setup of samples (and subsequently less operator-intensive data processing and
interpretation) should allow the mineralogist more time to solve complicated problems
associated with mine, processing plant, or exploration surveys.
Some have speculated that X-ray microtomography may replace auto-SEMs in
the near future. This is unlikely. In all likelihood, XRMs will be treated in a comple-
mentary fashion with XRMs providing critical three-dimensional information to ores
through the mapping of attenuation coefficients, analogous to 2D BSE grayscales
(proportional to average atomic number), with these attenuation coefficients being
regularly compared, correlated, and validated with auto-SEM X-ray data. The main
impedances to XRMs completely replacing auto-SEMs (in the near future) are as
follows:
Their reliance on attenuation coefficients. One cannot directly gain access to X-ray informa-
tion within a core/sample. Just like auto-SEMs have overlapping BSE grayscales between
minerals, XRMs have overlapping attenuation coefficients. So only in very simplistic sam-
ples would it be possible to separate minerals in an ore through attenuation coefficients.
Once a suitable attenuation coefficient of a specific value has been identified, one would
188 Iron Ore
still have to figure out exactly what mineral is being looked at through nondestructive means
(commonly by using an auto-SEM).
Price. XRMs are currently far more expensive than auto-SEMs.
Memory. The data created by XRMs are currently prohibitively large for large-volume scans
(gigabytes of data produced at approximately tens of micron resolution for approximately
cm3 volumes).
Resolution. XRM resolution is generally low (also to do with the size of data created by an
analysisthe higher the resolution, the more prohibitive the memory usage).
There is however much scope for XRMs being used in a complementary fashion
to auto-SEMs.
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