Chapter 6

Geometallurgical Characterization and

Automated Mineralogy of Gold Ores
J. Zhou1 and Y. Gu2
1
Joe Zhou Mineralogy Ltd, Peterborough, Ontario, Canada; 2Yingsheng Technology, Darra, Queensland, Australia

1. INTRODUCTION
The mining industry is a business full of risks, requiring substantial long-term investment. One of the risks is the technical
risk associated with project evaluation, process development, plant design, mine planning, and performance of mineral
processing/metallurgical unit operations, which is mainly caused by ore variability. To minimize and reduce the technical
risk, mining companies have been using geometallurgy in the past two decades to measure and quantify the spatial
variability of the deposits that are being developed. Geometallurgy is an interdisciplinary approach that links the
geological, geochemical, and mineralogical characteristics to the metallurgical performance of an orebody. Combined with
mine planning, it has been used in scoping, prefeasibility and feasibility studies, process design, and optimization of gold,
copperegold, copperemolybdenum, nickel and iron projects, among others (Williams and Richardson, 2004; Dobby et al.,
2004; Bulled, 2007; Bulled et al., 2009; Lotter et al., 2013; Kormos et al., 2013; Muinonen et al., 2013; Leichliter and
Larson, 2013; Leichliter et al., 2013; Hatton and Hatfield, 2013; Baumgartner et al., 2011, 2013; Hoal et al., 2013; Zhou,
2013). The goal of a gold or copperegold geometallurgical program is to characterize and understand the metallurgical
variability of an orebody, such as comminution, gravity, flotation, and cyanidation parameters and metal recoveries, and to
build a “geomet” model that can be used to assist in mine planning and to predict plant performance. In any geo-
metallurgical program, representative sampling is the key to ensure that the results of a geometallurgical study will reflect
future performance once the plant is commissioned. Mineralogical characterization and metallurgical testing, which leads
to an understanding of the orebody, lies at the core of a geometallurgical program. Geometallurgy complements, but does
not replace, the traditional mineralogical and metallurgical approach during the development and operation of a gold or
copperegold project. Geometallurgy is a methodology for test work design and a framework for mine planning. The first
part of this chapter provides an overview of geometallurgy fundamentals and application in gold ore processing, with a
focus being on ore characterization.
As a powerful tool in ore characterization, automated mineralogy has been used widely by the minerals industry and
research institutes for more than two decades and is commercialized in the form of techniques such as mineral liberation
analysis (MLA), QEMSCAN, and more recently Advanced Mineral Identification and Characterisation System (AMICS).
It generally uses scanning electron microscopy (SEM) hardware as a platform, combined with electron-dispersive
spectroscopy (EDS), and sophisticated software, to provide information on mineral speciation, composition, liberation,
association, and size distribution, etc. This information is not only required for new flowsheet development and process
selection but is also useful for plant optimization. The second part of this chapter will first provide an overview of the
basic functions of an automated SEM/EDS system, from sample preparation, to measurement, data processing and
reporting, introducing model analysis and liberation analysis as basic results. Then, methods especially related to
automated gold mineralogy analysis, such as bright/rare phase search (BRPS) and sparse phase liberation (SPL), are
discussed.

Gold Ore Processing. Mike D. Adams (Editor), http://dx.doi.org/10.1016/B978-0-444-63658-4.00006-2 95

Copyright © 2016 Elsevier B.V. All rights reserved.
96 PART | I Project Development

2. GEOMETALLURGY OVERVIEW
2.1 Definition
Geometallurgy is regarded as a new science in the area of economic mineral extraction. It is difficult to know when exactly
geometallurgy emerged and when the term was first framed, but certainly it appears to have evolved in the late 1980s or
early 1990s. However, real emergence of the study of geometallurgy dates mostly from 2000 and on (Hoal, 2008;
Williams, 2013). There are various, but essentially the same, definitions for geometallurgy, as follows:
l Geometallurgical mapping is a team-based approach that documents variability within an orebody and quantifies the
impact of geology (host rocks, alteration, and structure) and mineralogy on grinding, metallurgical response, and metal
recovery processes. It is an important tool to reduce the technical risk associated with new mine developments or ex-
pansions (Williams and Richardson, 2004).
l The geologically informed selection of a number of test samples to determine metallurgical parameters and the distri-
bution of these parameters through an orebody using an accepted geostatistical technique to support metallurgical pro-
cess modeling (SGS, 2013).
l An integrated, multidiscipline approach to the collection and modeling of geometallurgical information (Baumgartner
et al., 2011).
l A cross-discipline approach in which metallurgical performance of an ore is linked to intrinsic geological and miner-
alogical characteristics (Kormos et al., 2013).
l A scientific discipline in which geological data, mining data, and processing data are coanalyzed to generate useful
information and knowledge to optimize resource profitability (David, 2013).
l An interdisciplinary approach that links the geological, geochemical, and mineralogical characteristics to the metallur-
gical performance of an orebody. It is a framework and methodology for process design, mine planning, and plant opti-
mization (Zhou, 2013).
Figure 6.1 shows the links between important disciplines and their roles in geometallurgy.

2.2 Objective
Orebodies are naturally occurring phenomena with little consistency and similarity between different locations
and ore types. Even within a single orebody, rock types, ore grade, chemistry, mineralogy, alteration, and deportment
of payable metals and deleterious elements often change vertically and laterally, thus causing issues during ore
processing.
The objective of geometallurgy is to identify and understand the orebody variability and characterize its metallurgical
performance, including factors such as comminution, gravity, flotation and leaching parameters, and metals recoveries,
and to build a geometallurgical model that can be used to reduce the technical risk at the various stages of a mineral
project.

FIGURE 6.1 Various disciplines of importance in geometallurgy. Adapted from Williams and Richardson (2004) and this chapter.
 Geometallurgical Characterization and Automated Mineralogy of Gold Ores Chapter | 6 97

Overall, geometallurgy incorporates the principles of process mineralogy and material characterization as a tool for
predictive metallurgy. It complements, but does not replace, the traditional metallurgical approach during the project
development and mine operation. It mainly focuses on sampling, test work planning, and data integration.

2.3 Application
Geometallurgy has been used at all major stages of a range of mineral projects, including scoping, prefeasibility and
feasibility studies, process design and optimization, spanning gold, copperegold, copperemolybdenum, nickel, and iron
projects, during the past two decades. It plays an increasingly important role in the following aspects:
l Flowsheet development
l Equipment selection
l Mine planning
l Plant design and optimization
l Production prediction
As an interdisciplinary approach, geometallurgy links the geological, geochemical, and mineralogical characteristics to
the metallurgical performance of an orebody. It uses the geological information as a foundation and geostatistics as a tool
to collect samples from representative ore types with various grades, host rocks, and alterations at different locations of an
orebody and then conducts a comprehensive mineralogical and metallurgical test work on these samples to generate a large
amount of data. The data will be processed and integrated with other information and then imported into the geological
model to ascertain the distribution and variation of the mineralogical and metallurgical parameters within an orebody. Such
a geometallurgical model is then used for process selection, flowsheet development, mine planning, and plant optimization.
In recent years, geometallurgy has been advanced rapidly due to the need for developing a number of large deposits
(particularly gold ores) and to the implementation of some sophisticated analytical techniques such as mineral liberation
analyzer (MLA), QEMSCAN, dynamic secondary ion mass spectrometry (D-SIMS), time-of-flight secondary ion mass
spectrometry (TOF-SIMS), etc. (Dobby et al., 2004; Williams and Richardson, 2004; Baumgartner et al., 2011, 2013;
Lotter et al., 2013; Kormos et al., 2013; Leichliter and Larson, 2013; Leichliter et al., 2013; Zhou, 2013).

2.4 Approach
Geometallurgical programs require a team approach across the entire program and each individual component. A geo-
metallurgical program usually starts from geological investigation, including information collection and analysis, followed
by geological modeling. Based on the geological model, a geometallurgical matrix will be developed to guide sampling
and compositing for further testing. The most important part of a geometallurgical program is ore characterization,
including mineralogical studies and metallurgical test work. Overall, ore characterization is the quantification of physical
data on samples (drill cores and composites) that represent an orebody and provide criteria for process design and flowsheet
development. Figure 6.2 shows the flowsheet of a typical geometallurgical approach and Figure 6.3 shows the sampling
matrix for a geometallurgical program undertaken at Canahuire Au-Cu-Ag deposit in southern Peru. More information on
geometallurgical approach can be found in the reference papers.

3. GEOMETALLURGICAL CHARACTERIZATION OF GOLD ORES

Unlike base metal ores, which are usually processed using froth flotation, gold ores are often treated using several
processes in combination, including unit processes such as gravity separation, flotation, and cyanidation. For refractory
gold ores, in which gold occurs mainly as submicroscopic gold in sulfide minerals and is associated with carbonaceous
matter in some deposits, pretreatment is required before leaching, making gold ore processing more challenging and ore
characterization more important.

3.1 Classification of Gold Ores and Minerals

3.1.1 Gold Ore Types
Gold ores are commonly classified into two major categories: free-milling and refractory. Typically, free-milling ores are
defined as those where over 90% of gold can be recovered by conventional cyanide leaching. Refractory ores are defined as
98 PART | I Project Development

Geological investigation
(Foundation)

Geomet matrix establishment

(Framework)

Sampling & Compositing

(Key)

Ore characterization
(Core)

Geomet modelling
(Integration)

Process design Mine planning & Plant

& Engineering Production forecasting optimization

FIGURE 6.2 Simplified flowsheet illustrating typical geometallurgical approach.

FIGURE 6.3 Sampling matrix including lithology, alteration, and mineralization at Canahuire Au-Cu-Ag deposit. Domains are shown in colors,
while samples taken for the geometallurgical study are shown in tan. Note that some of the 51 samples are comprised inside the cube and thus are not
visible. Parts that are not sampled indicate that the combination of the three variables does not exist or that samples were not available. After Baumgartner
et al. (2011).
 Geometallurgical Characterization and Automated Mineralogy of Gold Ores Chapter | 6 99

1. Placers
2. Quartz vein-lode ores
3. Oxidized ores

More free-milling
4. Silver-rich ores

More refractory
5. Copper sulfide ores
6. Iron oxide copper-gold ores
7. Iron sulfide ores
8. Arsenic sulfide ores
9. Antimony sulfide ores
10. Bismuth sulfide ores
11. Telluride ores
12. Carbonaceous sulfide ores
FIGURE 6.4 Classification of gold ore types. Adapted from Zhou et al. (2004), Marsden and House (2006), and this chapter.

those that yield low gold recoveries or result in acceptable gold recoveries only with significantly higher reagent con-
sumptions or more complex pretreatment processes (La Brooy et al., 1994; Zhou et al., 2004; Marsden and House, 2006).
Prior to 1980, all gold plants treating refractory ores first concentrated the gold-bearing portion of the ore by flotation and
then roasted the float concentrate to convert the sulfides to SO2 gas and produce a hematite calcine. Gold recovery from the
calcine by conventional cyanidation and MerrilleCrowe zinc cementation was typically in the 80e90% range. New
technologies of pressure oxidation (POX) and bioleaching were developed and implemented after 1980. These processes
offered a clean alternative to the toxic gases (SO2 and As2O3) that were released to the atmosphere during roasting and
generally resulted in improved gold recovery (typically 90e98%) (Deschênes et al., 2011).
Based on the mineralogical characteristics and mineral processing techniques required, gold ores can be classified into
12 types, depicted in Figure 6.4. Generally speaking, the first six gold-ore types in Figure 6.4 are more free-milling and the
other six ore types are more refractory, and from top to bottom, the refractoriness increases. Carbonaceous sulfide ores are
regarded as the most difficult ores to treat due to the presence of carbonaceous matter and submicroscopic gold. This type
of ore needs to be pretreated before gold extraction to achieve acceptable gold recoveries.

3.1.2 Gold Mineralogical Types

Mineralogically, gold in an ore or mill product can be classified into three forms based on its deportment: microscopic
gold, submicroscopic gold, or surface gold. Microscopic gold, also known as visible gold, comprises all microscope-visible
gold minerals such as gold alloys, gold tellurides, gold sulfides, gold selenides, gold sulfotellurides, and gold sulfosele-
nides. Microscopic gold is found in many gold ores and is the main form of gold in nonrefractory gold ores. Gold that is
invisible under optical and scanning electron microscopes is referred to as submicroscopic gold (or invisible gold) and is
the major form of gold in refractory gold ores such as Carlin-type gold deposits, some epithermal gold deposits, and
volcanogenic massive sulfide (VMS) deposits. Surface gold is gold that was adsorbed onto the surface of other minerals
(such as carbonaceous material and iron oxide) during mineralization and subsequent oxidation or metallurgical
processing.
Gold minerals in this chapter are defined as the minerals in which gold is present as a main constituent (e.g., native
gold and electrum). Gold carriers are defined as both the gold mineral and the mineral in or on which gold occurs
in minor or trace amount (such as pyrite and arsenopyrite). Figure 6.5 lists the three forms of gold and some common
gold minerals and carriers. More information on the definition of and an introduction to the gold forms and carriers can
be found in a number of publications (Zhou et al., 2004; Marsden and House, 2006); refer also to Chapter 5 of this
volume.

3.2 Ore Characterization

Ore characterization may be defined as the quantification of physical data on samples that represent an orebody. Data
collected as part of an ore characterization program provide the objective foundation for a sound geometallurgical
approach. Unlike geometallurgical mapping, ore characterization has no spatial references (Williams and Richardson,
2004). Table 6.1 lists some possible tests required in ore characterization for a geometallurgical program.
100 PART | I Project Development

FIGURE 6.5 Classification of gold by forms and carriers.

TABLE 6.1 Tests That Quantify Various Parameters Important in Ore Characterization

Discipline Parameter Testing Possible

Geology Field relationships Mapping, drilling, decline
Geochemistry Grade of valuable and deleterious elements; Assays
whole-rock analysis
Mineralogy Zonation, deportment of payable metals and Mineral identification, association, grain size, textural and
deleterious elements liberation data all available via AMICS, QEMSCAN, MLA,
D-SIMS, TOF-SIMS, and other instruments
Physical Hardness e grinding Bond work indices, JK drop-weight test, semiautogenous
properties grinding power index, MacPherson 18-in. mill test
Metallurgical Recovery, concentrate grade, reagent dosage Flotation kinetics, locked-cycle tests, gravity-recoverable
response gold, bottle rolls

Geotechnical Site preparation, environmental review Soil density, ground water flow, slope stability
measures

Adapted from Williams and Richardson (2004).

3.3 Impact of Mineralogy on Gold Ore Processing

The extractive metallurgy of gold ores is largely driven by mineralogical factors due to the fact that gold often occurs in at
least two forms in an ore. These factors include particle size, association with other minerals, coatings and rimmings,
presence of cyanicides, oxygen consumers and preg-robbers, presence of refractory gold minerals and locking of sub-
microscopic gold in sulfide and sulfarsenide mineral structures, etc. Table 6.2 lists some common mineralogical issues and
the processing technologies that may be affected in gold ore processing.
Among the factors listed in Table 6.2, liberation, grain size and association are regarded as the top three factors that
are seen in all gold ores and must be characterized in a geometallurgy program. Presence of refractory gold minerals such
as gold tellurides such as calaverite [AuTe2] and sylvanite [(Au,Au)Te2], aurostibite [AuSb2], and maldonite [Au2Bi]
often cause lower gold recoveries due to their slow leaching kinetics. Submicroscopic gold and carbonaceous matter
 Geometallurgical Characterization and Automated Mineralogy of Gold Ores Chapter | 6 101

TABLE 6.2 Common Mineralogical Issues Affecting Gold Extraction

# Mineralogical Issue Affected Processes

1 Liberation/locking Gravity, flotation, and leaching
2 Grain size Gravity, flotation, and leaching
3 Association Gravity, flotation, and leaching
4 Surface chemistry Gravity, flotation, and leaching
5 Coating and rimming Gravity, flotation, and leaching
6 Dissolution kinetics Leaching
7 Cyanicides and oxygen consumers (secondary copper minerals, Leaching
pyrrhotite)
8 Refractoriness (submicroscopic gold) Gravity, leaching
9 Preg-robbing (C-matter, iron oxide, etc.) Leaching
10 Deleterious minerals/toxic elements (As, Hg, Se, Sb, Te, etc.) Flotation, leaching, solution purification, and tails
disposal
11 Gangue mineralogy (clays, acid-forming and acid-consuming Flotation, leaching, and tails disposal
minerals)

Updated from Zhou (2013).

are the major trouble-makers in carbonaceous sulfide ore processing, where gold is not only locked in sulfide minerals
but also absorbed onto carbonaceous matter during leaching (preg-robbing). More information on how mineralogical
factors affect gold extraction can be found elsewhere (Zhou et al., 2004; Zhou, 2013), as well as in Chapter 5 of this
volume.

3.4 Gold Deportment Study

Gold deportment study is critical to any gold project and the information generated from such a study can be used for
assisting in process selection and flowsheet development. To properly and precisely determine the deportment of gold in an
ore or mill product, some comprehensive approaches involving advanced and conventional techniques have been devel-
oped and used for gold deportment studies (Chryssoulis and Cabri, 1990; Wang et al., 1994; Butcher et al., 2000; Zhou
et al., 2004; Zhou, 2013); see also Chapter 5. Compared to other procedures using a single technique and a small quantity
of sample, the advantages of using these comprehensive approaches are that a large sample will be studied to improve
statistics, and each issue will be addressed properly using specific techniques.

3.4.1 Investigative Procedure

Figure 6.6 illustrates a simplified study procedure for gold deportment used at JZMIN, including characterization of
microscopic gold, submicroscopic gold, and surface gold. High-grade and free-milling ore deposits (gold ores that give a
gold recovery >90% with an 80% <75-mm grind and 20e30 h conventional cyanidation leach) (La Brooy et al., 1994) are
becoming depleted. More low-grade and refractory ores are being discovered and processed. As a result of these trends,
submicroscopic gold is becoming more common and now accounts for a significant portion of many gold ores. In gold ores
containing carbonaceous material, gold extraction can be challenged by its preg-robbing nature. Therefore, characterization
of submicroscopic gold must be considered for those ores yielding low gold recovery by conventional cyanide leaching.
The preg-robbing capacity of carbonaceous matter needs to be investigated for gold ores showing preg-robbing potential,
to evaluate the impact of gold deportment and other mineralogical issues on gold extraction. As shown in Figure 6.6, a gold
deportment study program usually starts from microscopic gold to determine the speciation, composition, quantity,
liberation, association, and particle size distribution of gold minerals. Based on the acquired information, estimation of
gold recovery by gravity, flotation, cyanidation, or a combination of these techniques can be established. If microscopic
gold accounts for 80% or less, characterization of submicroscopic gold is recommended. Surface gold analysis is only
considered when the ore shows preg-robbing potential.
102 PART | I Project Development

Chemical Crushed ores Modal

analysis (Mill products) mineralogy

Refractory? Gold Preg-robbing?

Deportment

Identification and Speciation & Identification and

quantification of Composition quantification of
submicroscopic gold preg-robbers &
carriers & varieties surface areas
Liberation &
Association

Quantification of Quantification of
submicroscopic gold Size distribution surface gold
of gold & host

Distribution of Estimation of Distribution of

submicroscopic gold gold recoveries surface gold

Gold mineralogical balance

Evaluation of mineralogical factors affecting recovery
Recommendation for process selection or optimization

FIGURE 6.6 Simplified investigation procedure for gold deportment. Adapted from Zhou (2013).

3.4.2 Commonly Used Techniques

Gold deportment study, particularly detection and quantification of submicroscopic gold and surface gold, requires the use
of sophisticated analytical techniques. To address each mineralogical issue effectively and efficiently, a number of
advanced and conventional techniques have been used in gold deportment studies (Table 6.3). Commonly used techniques
include optical microscopy, SEM, D-SIMS, and TOF-SIMS (Chryssoulis and Cabri, 1990; Wang et al., 1992; Dimov et al.,
2003; Zhou et al., 2004; Cabri and Jackson, 2011); also refer to Chapter 5. Due to the extremely low concentration of gold
in the samples to be studied (particularly tailings samples of various types), preconcentration techniques such as heavy-
liquid separation, tabling, and superpanning are often used to improve the efficiency and representativeness of the
technique.
In recent years, advanced techniques have gained significant development and played an important role in gold
mineralogical study such as the use of QEMSCAN alongside traditional diagnostic leaching in the characterization of
visible gold in complex ores (Goodall et al., 2005). However, it should be noted that conventional techniques, such as
optical microscopy and preconcentration, are still important techniques in gold deportment study and will not be
substituted by advanced techniques in the foreseeable future. In a gold deportment study, optical microscopes can be used
not only for gold scanning and bulk mineralogical examination but also for sample preparation required by a number of
instruments. For example, target minerals must be identified and carefully selected under microscope before they are
analyzed for submicroscopic gold concentration by SIMS or other microbeam techniques. In addition, the abundance and
textural types of gold carriers need to be determined under a microscope so that this information can be used in calculating
the cumulative gold concentration in target minerals. It is the same for surface analysis e before quantifying the surface
gold adsorbed on carbonaceous material or other mineral grains, these mineral grains must be identified and carefully
selected under microscope. If the samples are not properly prepared, all subsequent instrumental analyses will become less
meaningful, useless, or even misleading. Sample preparation is also critical for surface studies to detect and quantify
collectors or depressants on the surface of valuable or gangue minerals. Samples for surface analysis are very sensitive and
cannot be exposed to any electron, proton, or X-ray beams prior to surface analysis. These samples, often individual
particles, must be carefully selected and prepared under optical microscopes from as-received samples to avoid changing
the surface composition (Zhou, 2013).
 Geometallurgical Characterization and Automated Mineralogy of Gold Ores Chapter | 6 103

TABLE 6.3 Techniques Commonly Used in Gold Deportment Study

Category Technique Abbreviation Application MDL

Qualitative/ Optical microscopy OM Mineral ID and qualitative/semiquantiative High
semiquantitative mineral analysis of bulk material (%)
Semiquantitative Automated digital image system ADIS Mineral ID and qualitative/semiquantitative High
mineral analysis of bulk material (%)
X-ray diffraction XRD High
(%)
Scanning electron microscopy SEM Mineral ID and qualitative/semiquantitative High
elemental analysis of individual particle (%)
Quantitative Mineral liberation analyzer MLA Quantitative mineral analysis of bulk Low
samples and individual particle (%)
Quantitative evaluation of QEMSCAN Low
materials by scanning electron (%)
microscopy
Quantitative Electron probe microanalysis EPMA Quantitative elemental analysis of Low
individual particle (ppm)
Proton-induced X-ray emission PIXE Low
(ppm)
Dynamic secondary ion mass D-SIMS Low
spectrometry (ppm e
ppb)
Laser ablation microprobe LAM-ICP-MS Low
einductively coupled plasma (ppm e
emass spectrometry ppb)
Surface analysis Time-of-flightelaser ion mass TOF-LIMS Surface analysis of bulk material and Low
spectrometry individual particle (ppm)
Time-of-flightesecondary ion TOF-SIMS Low
mass spectrometry (ppm)

X-ray photon spectrometry XPS Surface analysis of bulk material Low

Updated from Zhou et al. (2004).

3.4.3 Deliverables
Gold deportment study is an important part of geometallurgy program. It is becoming a powerful tool in predicting the
metallurgical performance of a new ore and in troubleshooting the gold loss in an operating plant. If the test work is well
designed and properly executed, a gold deportment study will provide very useful information on process selection,
flowsheet development, recovery improvement, and reagent-consumption optimization. The results acquired from such a
study program should be able to reflect future metallurgical performance of a new ore or identify the cause(s) for gold
losses. To ensure that a gold deportment study will provide correct and accurate information as required, selection of
mineralogical techniques is most important for any gold project. It is recommended that a comprehensive mineralogical
investigation procedure involving conventional and advanced techniques (Figure 6.6 and Table 6.3) be used for such
studies. Deliverables of a typical gold deportment study include the following information.
l Liberated gold: recoverable by gravity, flotation, or cyanidation;
l Gold associated with sulfide minerals: recoverable by flotation with/without cyanidation or noncyanide leaching;
l Gold associated with nonsulfide minerals: partially recoverable by leaching. Locked gold is nonrecoverable unless fine-
grinding is involved;
l Preg-robbing capacity of carbonaceous matter: to be pretreated by roasting or autoclaving, if present; and
l Mineralogical factors that may affect or have affected gold extraction.
104 PART | I Project Development

4. AUTOMATED MINERALOGY OF GOLD ORES

4.1 Background
Optical microscopy has been a very important tool for mineral identification and quantification. It can be automated to gold
search or to obtain quantitative mineral composition of rock and ore specimens. However, it lacks the ability to obtain
elemental composition, which can vary significantly in a large number of minerals. When SEM became available in the
1960s, mineralogists quickly embraced it. Significant efforts were made to automate it for quantitative mineral analysis
(Hall, 1977; Grant et al, 1977; Jones, 1987). Its value as a tool for process mineralogy was soon demonstrated (Jones,
1987; Sutherland et al., 1988). When the SEM/EDS hardware and computing power and speed sufficiently improved in the
1990s, automated SEM for mineral analysis became an important technique used widely by the minerals industry and
research organizations alike.
The first generation of SEM-based tools were developed in Canada (MP-SEM-IPS at CANMET), in Finland (at VTT),
in UK (Imperial College London), in South Africa (ASCAN at Anglo Research), and in Australia (QEM*SEM
and CCSEM). The QEM*SEM was further developed into QEMSCAN by CSIRO and Intellection in Australia (Gottlieb
et al., 2000). The Mineral Liberation Analyzer (MLA) was developed at JKMRC using the latest hardware and software
technology at the time in the late 1990s (Gu, 2003). Recent developments include the TESCAN Integrated Mineral
Analyzer (TIMA) in the Czech Republic (Králová, 2012; Králová and Dosbaba, 2014; Khajehpour and Králová, 2014) and
the Advanced Mineral Identification and Characterization System (AMICS) by Yingsheng Technology from Australia.
This section will first provide an overview of the basic functions of an automated SEM/EDS system, from sample
preparation, to measurement, data processing and reporting, introducing model analysis, and liberation analysis as basic
results. Then, methods especially related to automated gold mineralogy analysis, such as B/RPS and SPL, are explained.

4.2 System Hardware Requirement

The two main hardware components are SEM and energy dispersive X-ray spectroscopy (EDS, EDX, or XEDS).
Figure 6.7 shows an example of the type of hardware typically required for automated mineralogy systems, including
QEMSCAN, MLA, and in the example shown, an AMICS system. The SEM and EDS systems are usually controlled by
different computers linked by Ethernet cables. Since a large number of EDS X-ray points are normally analyzed during
data acquisition, X-ray acquisition is usually the most time-consuming part of the online measurement step. Hence,
multiple EDS detectors are sometime used to accelerate the X-ray collection.
Requirements for the SEM system are:
1. Computer-controlled specimen stage for automated movements in at least x and y directions
2. Stable beam for extended period (24 h) of unattended operation
3. Very good back-scattered electron (BSE) image for mineral gray-level separation
4. Strong enough beam to produce high rate of X-rays in mineral samples

FIGURE 6.7 An example of the type of hardware typically required for automated mineralogy systems, including QEMSCAN, MLA, and in the
example shown, a standard AMICS set up with Hitachi SU3500 and Bruker 630 EDS detector.
 Geometallurgical Characterization and Automated Mineralogy of Gold Ores Chapter | 6 105

Requirements for the EDS system are:

1. High count rate (200,000 cps) throughput at reasonable resolution (135e140 eV) and low dead time (<30%)
2. Allow for flexible control single or multiple X-ray collection
3. Allow for multiple detectors working together
4. Be able to control SEM for imaging (external scan)

4.3 Sample Selection and Preparation

Samples for gold analysis usually come from (1) processing plant (granulated sample) or (2) mine or prospects (rock chips
or drill cores). Granulated samples can be preconcentrated and sized to fractions. Rock chips or drill cores can be crushed
to 0.5e1 mm or finer for subsampling. It usually needs to take a large sample to ensure the representativeness. For
complete analysis, each fraction will be analyzed. The selected samples for analysis are usually mounted in epoxy resin of
25- or 30-mm-diameter blocks or normal glass slides (Figure 6.8). Sometimes, square blocks are used to maximize the area
available for analysis. The mounted surface is cut, polished, and coated with carbon before presented to the SEM for
analysis.
It was found that when the sample particles are fine (
53 mm), they need to be double mounted to get representative
results. Figure 6.9 shows the measured settling profile of a double-mounted sample. It clearly shows that the bigger and

FIGURE 6.8 Prepared samples for quantitative gold mineralogy analysis.

FIGURE 6.9 A BSE image showing typical settling profile of a granulated sample.
106 PART | I Project Development

heavier particles are concentrated at the bottom surface of the first mount step. A vertical cut is made to the first mount
sample block and the cut surface is used for observation after the second mount step.
Also, fine particles tend to agglomeration during the sample preparation, so graphite particles are sometimes mixed with
sample particles during sample preparation to minimize agglomeration.

4.4 Basic Measurements

There are two basic measurements in a quantitative mineralogy system: (1) point analysis, which produces mineral
abundance, and (2) area analysis, which produces liberation and association, grain size distribution for each mineral, as
well as mineral abundance.
Point analysis is the equivalent of traditional point counting using optical microscopy. In this type of analysis, the BSE
image is first taken to differentiate between background and mineral particles of interest. X-ray points are located on
particles based on user-selected grid spacing. For each grid point, one X-ray spectrum is collected and mineral identity
determined (see Figure 6.10).
In point analysis, the number of counts for each mineral accumulated is proportional to its volume percent in a sample.
Table 6.4 shows a sample output of point analysis. The relative error equals 2  standard deviation (s) above and below
the measured value at 95% confidence level (Jones, 1987).
The measured mineral abundance data can be used to calculate the bulk chemical composition of the sample using
density and elemental composition of the minerals involved. This calculated assay is often compared with independent wet
chemistry assay of the same sample.
Area analysis produces a mineral map of the measured sample surface and a set of mineral statistics, such as mineral
liberation and association and grain size distribution, etc. This type of analysis starts with BSE image acquisition and based
on the gray-level variation in the image determines possible mineral grain domains for X-ray collection and mineral
identification. This process is schematically shown in Figure 6.11.
Liberation and association data can be generated from mineral map. To obtain accurate liberation data, each plant
sample is sized into different size fractions and measured separately. This is to reduce the stereological bias that is
inevitable when attempting to measure three-dimensional objects with their two-dimensional sections (Spencer and
Sutherland, 2000; Keith, 2000; Lätti, 2006).
Area analysis with X-ray mapping is the other method commonly used to perform liberation analysis of samples from
mineral processing plant. In this method, BSE image is acquired and particle masks are generated by removing the
background. For each particle mask, an array of points is placed over it and one X-ray spectrum is obtained for each point
and its mineral identity determined. Thus, a mineral map is generated for every particle. This process is shown in
Figure 6.12.

FIGURE 6.10 Illustration of point analysis and mineral identification.

 Geometallurgical Characterization and Automated Mineralogy of Gold Ores Chapter | 6 107

TABLE 6.4 Mineral Abundance Produced by Point Analysis

Relative Error
Name Weight (%) Area (%) Area (mm2) Points Estimates (%)
Quartz 25.87 44.57 3710.72 1017 5
Alloclasite 23.92 12.49 1039.88 285 11
Pyrrhotite 19.72 14.77 1229.61 337 10
Pyrite 7.71 5.3 441.49 121 18
Dolomite 7.22 8.76 729.74 200 14
Feldspar 5.2 6.84 569.2 156 15
Galena 5.08 2.37 197.03 54 27
Chalcopyrite 2.72 2.23 186.08 51 28
Sphalerite 1.03 0.88 72.97 20 45
Biotite 0.83 0.92 76.62 21 43
K-feldspar 0.2 0.26 21.89 6 82
Apatite 0.19 0.22 18.24 5 89
Chlorite 0.12 0.18 14.59 4 100
Fluorite 0.11 0.13 10.95 3 115
Rutile 0.04 0.04 3.65 1 200
Calcite 0.04 0.04 3.65 1 200
Total 100 100 8326.31 2282

FIGURE 6.11 Area analysis using both BSE and X-ray: top left is the original BSE image; top middle is the corresponding mineral map; top right is the
BSE image of a particle; bottom left is its segmented image with X-rays; bottom middle is its mineral map; and bottom right is the color index/legend of
the mineral map. In the segmented image of the particle, each domain is represented by a color and there is a “þ” symbol, which indicates that an X-ray is
acquired at that point. The particle is about 80 mm (in width).
108 PART | I Project Development

(a) (b) (c)

FIGURE 6.12 Area analysis with X-ray mapping: (a) original particle BSE image; (b) X-ray grid, of 4 mm spacing, placed over particle mask;
(c) mineral map generated from X-ray points, showing a quartz grain mostly enclosed by albite. The particle is 200 mm. Quartz/albite sample kindly
provided by Mr. Jukka Laukkanen of Geological Survey of Finland.

This method does not rely on the gray-level separation between different minerals present, so it was a good choice in
the 1970 and 1980s when the typical BSE detector produced low-quality images. One important disadvantage of this
method is that it requires a lot more X-ray points to outline the mineral grains in a particle. Thus, systems based on this type
of analysis usually require up to four EDS detectors.

4.5 Advanced Features

Development of both hardware and software features of both MLA and QEMSCAN has taken place since the first
prototypes were tested (Gottlieb et al., 2000; Gu, 2003); these technologies are now both marketed by FEI (2016).
A recent development in the AMICS system, called fine segmentation method, aims to combine the two area analysis
methods presented earlier. In this method, the user adjusts the level of segmentation to control the size of each segment.
Segment size can be as small as the X-ray spacing step, or as large as in the standard area analysis, where only phases with
clearly different gray levels will be separated. This process is shown in Figure 6.13.
Note that there is virtually no difference in BSE gray level between quartz and albite in this sample. Yet, it can be seen
that this method produced almost the same result as from the X-ray mapping method, with a much lower number of X-ray
points being used.

4.6 Gold and Rare Phase Search

Since the concentration of gold and other precious metals in most samples are very low (at ppm level), it would be very
hard to obtain statistically valid data using normal area or point analysis methods. In an average ore with 5 ppm gold
(by weight), the volume grade of gold is about 1 ppm since the density of gold is around 5e6 times the bulk density of
the ore. To measure such a sample, we would need to analyze 1 million particles to see one gold particle, if the average
size of gold particle is the same as others. In order to efficiently measure this type of sample, one approach is to scan
each field quickly first to determine if there is a possibility that this field contains gold based on the BSE brightness
distribution. If so, X-ray analysis is performed on areas of interest and the data is saved for mineral identification.
This method is so-called RPS.

(a) (b) (c)

FIGURE 6.13 Fine segmentation method: (a) original particle BSE image; (b) segmented image with one X-ray point per segment; (c) mineral map
generated, showing the very similar result as in X-ray mapping method illustrated in Figure 6.6, with a third of X-ray points. Quartz/albite sample kindly
provided by Mr. Jukka Laukkanen of Geological Survey of Finland.
 Geometallurgical Characterization and Automated Mineralogy of Gold Ores Chapter | 6 109

FIGURE 6.14 Example of output from RPS. Particles BSE image showing Au and Ag tellurites, the bright inclusions, in pyrite particles.

Since this method is focused on minerals of interest and does not spend X-ray analysis time on common gangue
minerals, it is usually much quicker to accumulate enough statistics for gold than the area analysis and point analysis
methods. The output of the type of analysis is usually gold mineral types, their association with other minerals, their size
distributions, and images. Figure 6.14 shows some particles found with RPS measurement.

5. SUMMARY AND CONCLUSIONS

Geometallurgy is an interdisciplinary approach that links the geological, geochemical, and mineralogical characteristics to
the metallurgical performance of an orebody. The objective of gold geometallurgy is to reduce and minimize the technical
risk in project evaluation, plant design, mine planning, and production forecasting through geometallurgical modeling,
representative sampling, and subsequent systematic mineralogical and metallurgical test work. Geometallurgy is a tech-
nique to document variability within an orebody and quantify and evaluate the impact of many factors including geology
and mineralogy on grinding, flotation, leaching, and metal recovery processes.
Automated mineralogy is an important technique used widely by the minerals industry and research institutes in ore
characterization. It uses SEM hardware as a platform, combined with sophisticated software to provide information on
mineral speciation, composition, liberation, association, size distribution, and metal balance. It is a powerful tool in gold
deportment study that is often an important part of gold geometallurgy.

ACKNOWLEDGMENT
The authors are grateful to the editorial team for their encouragement and assistance in preparing this chapter. Anonymous reviewers are
acknowledged for their constructive comments, which helped to improve the manuscript. Companies that have contributed indirectly to this
chapter by providing projects and financial support are also acknowledged.

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Joe Zhou is a process mineralogist and geometallurgist with over 30 years’ experi-
ence in research and development, laboratory testing, and consulting for the minerals
industry. His career includes 22 years in Canada and Australia and 15 years in China
with a number of renowned research institutes, commercial laboratories, and mining
companies. He established Joe Zhou Mineralogy Ltd in Canada in early 2010 and has
been principal consultant and director for the company since then. He also holds a
position as executive deputy general manager and chief engineer at XZMMTC of
Zijin Mining Group in China. Joe is a licensed professional engineer in Canada. In
the past years, Joe was involved in several hundred projects for new deposits and
operating mines around the world, including all major types of base metal and
precious metal ores, and has authored or co-authored over 200 reports and over 40
publications. He developed and implemented the comprehensive methodology for
gold and silver deportment study at several research and commercial laboratories.

Dr Ying Gu studied geology and geochemistry at Nanjing University and Monash

University. He also obtained a degree in computer studies from Murdoch University.
Over the last 20 years, he worked exclusively in automated mineralogy research, as a
mineralogist at a mine and a researcher at CSIRO and then at the University of Queens-
land (1996e2015), where he led a research project that developed the Mineral Liber-
ation Analyzer (MLA), which is now widely used in research institutions and mining
companies worldwide. In recognition of his contributions to the successful develop-
ment and commercialization of the MLA, Ying received Innovation Heroes Award
in 2011 by The Warren Center for Advanced Engineering. He was president of the
ICAM from 2008 to 2011. He is now with Yingsheng Technology, Australia, devel-
oping and marketing the third-generation automated mineralogy tool, Advanced Mineral
Identification and Characterization System (AMICS), which represents the latest innova-
tion in this field of research.