2016 - D - Good Sampling Practice (MNT)

Mining Technology
Transactions of the Institutions of Mining and Metallurgy: Section A
ISSN: 1474-9009 (Print) 1743-2863 (Online) Journal homepage: http://www.tandfonline.com/loi/ymnt20
Importance of good sampling practice throughout

the gold mine value chain
S. C. Dominy
To cite this article: S. C. Dominy (2016) Importance of good sampling practice
throughout the gold mine value chain, Mining Technology, 125:3, 129-141, DOI:
10.1179/1743286315Y.0000000028
To link to this article: http://dx.doi.org/10.1179/1743286315Y.0000000028
Published online: 11 Mar 2016.
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Download by: [Australasian Institute of Mining and Metallurgy (AusIMM)]
Date: 20 June 2016, At: 16:52
Importance of good sampling practice

throughout the gold mine value chain
Downloaded by [Australasian Institute of Mining and Metallurgy (AusIMM)] at 16:52 20 June 2016
S. C. Dominy1,2
The mining industry routinely collects samples to assist with decision making, whether for exploration,
resource estimation, grade control, or plant design and balances. Poorly designed sampling protocols
can result in elevated project risk by increasing variability. Critically, such variability produces both
financial and intangible losses. Sample collection, preparation and assay or test work protocols that are
optimised to suit the ore type, together with QAQC systems will reduce variability. Many gold deposits
display a high natural variability, where the in situ variability can be enhanced by poor sampling practice
to yield a high-nugget effect. In this case, specialised protocols are often required. Reporting codes
require the Competent Person to consider the quality and implication of sampling programmes. Despite
its importance, sampling often does not receive the attention it deserves. In this paper, the importance of
good sampling practice is exemplified through a series of case studies, which show the many sampling
issues that frequently go unrecognised or unaddressed, resulting in poor decisions and financial loss.
Keywords: Theory of sampling, Sampling errors, Gold sampling, Protocol optimisation, Financial losses
Abbreviations
AAS
atomic absorption spectroscopy;
HARD half absolute relative difference;
ACE
accelerated cyanide extraction;
HT
heterogeneity test;
AE
analytical error;
HQ
diamond drill core (diameter of 63.5mm);
BH
blast hole drilling;
ISE
incorrect sampling error;
CH
constitution heterogeneity;
sampling constant;
CRM
Certified reference material;
NQ
diamond drill core (diameter of 48mm);
CSE
correct sampling errors;
PAL
pulverise and leach;
DH
distribution heterogeneity;
PE
preparation error;
DE
delimitation error;
QA/QC quality assurance/quality control;
gold liberation diameter;
RC
reverse circulation drilling;
EE
extraction error;
ROM
run of mine;
FA
fire assay;
FSE
sampling error;
SFA
screen fire assay;
GNE
geological nugget effect;
SNE
sampling nugget effect;
GRG
gravity recoverable gold;
TOS
theory of Sampling
GSE
grouping and segregation error;
Camborne School of Mines, University of Exeter, Penryn, Cornwall,

TR10 9FE, UK
2
Western Australian School of Mines, Curtin University, Bentley, WA,
6102, Australia
1
Email s.dominy@e3geomet.com
2016 Institute of Materials, Minerals and Mining and The AusIMM
Published by Taylor & Francis on behalf of the Institute and The AusIMM
Received 14 June 2015; accepted 4 August 2015
DOI: 10.1179/1743286315Y.0000000028
Introduction
The importance of high-quality sampling throughout the gold
mine value chain, from exploration, through evaluation and
exploitation, has been stressed by many authors (Carrasco,
Carrasco and Jara 2004; Dominy, Nopp and Annels 2004;
Gy 1982, 2004; Holmes 2004, 2015; Minnitt 2007, 2013;
Morrison and Powell 2006; Pitard 1993, 2009; Sketchley
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2016VOL. 125NO. 3
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Dominy Importance of good sampling practice
1998; Spangenberg 2011). The sampling process, inclusive

of sample collection, preparation and assaying or testing, is
a critical component to all stages of a mining project as it
forms the basis for Mineral Resource and Ore Reserve estimates (JORC 2012). Sampling includes in situ material and
broken (or crushed) rock for both geological and metallurgical
purposes. The focus is often on grade sampling (e.g. resource
definition and grade control), though metallurgical sampling
for plant design, control and metal balances (Giblett, Dunne
and McCaffery 2012; Guresin et al. 2012; Holmes 2004) must
not be ignored.
In all cases, the aim is to gain a representative sample to
accurately describe the material in question. Field sample
collection is followed by sample reduction in both mass and
fragment size to provide an assay charge or test sample. This
process is challenging in the gold environment and particularly when a high-nugget effect and/or coarse gold is present
(Dominy 2014a; Dominy, Johansen, Annels and Cuffley 2000;
Dominy and Petersen 2005; Pitard 2007; Royle 1989).
This contribution presents case studies that exemplify
some of the sampling issues that can be typically identified
across the gold mine value chain. The effects of poor practice are presented and solutions given. An attempt is made
to provide a financial and intangible loss estimate for each
case study.
Theory of sampling
Theory of sampling overview
Samples should be collected and prepared within the framework of the Theory of Sampling (TOS) (Gy 1982; Pitard
1993), along with an appropriate QAQC system (Sketchley
1998; Simon and Gosson 2010; Valle 1998). Sampling errors
are defined in TOS; the key errors are defined in Table 1 (Gy
1982; Pitard 1993). Uncontrolled errors lead to an elevated
nugget effect (Carrasco 2009; Dominy 2014a; Pitard 2007).
Theory of sampling was developed in the 1950s by Dr
Pierre Gy at the time to deal with sampling challenges in
the mining industry (Franois-Bongaron 2008; Gy 1982).
Its usage subsequently spread to other sampling applications
across the food, pharmaceuticals, environmental and waste
management sectors to name a few. Across the mining industry, its application has been highly variable though on the
increase since the late 1980s, but to date not routinely applied.
Over the last 15years, the author has had involvement with
around 120 gold projects globally, for which only around 20
could be said to be fully compliant with TOS.
Some authors have questioned the applicability of TOS
and in particular the so-called FSE equation applied to
gold (Geelhoed 2011). Franois-Bongaron (1998) and
Franois-Bongaron and Gy (2002) addressed key issues
and proposed a modified FSE equation. The modified
equation has been applied successfully by practitioners
to optimise sampling campaigns (Afewu and Lewis 1998;
Cintra et al. 2007; Cossio, Noyola, Gonzalez and Espinosa
2004; Dominy and Petersen 2005; Dominy, Platten, Xie and
Minnitt 2011; Fallon et al. 2012; Pitard 2009). The use of
the equation represents a modelled expectation that may or
may not be attained in practice, but provides a starting point
for optimisation.
Beyond the FSE equation, TOS provides important guidelines for reducing the sampling errors (Table 1). It is here to
stay, though there is still much to do in context of research,
communication and education (Franois-Bongaron 2008,
2015; Pitard, Esbensen and Paoletti 2015).
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Nugget effect and TOS

The nugget effect is the random component of variability
that is superimposed on the regionalised variable, and is
defined in a variogram as the percentage ratio of nugget
variance to total variance. The magnitude of the nugget
effect relates to: in situ heterogeneity of the mineralisation;
sample support; sample density; and sample and assay procedures (Carrasco 2009; Franois-Bongaron 2004; Pitard
2007).
The nugget effect has two principal components (Carrasco
2009; Dominy 2014a; Franois-Bongaron 2004; Pitard 2007;
Platten and Dominy 2003): the geological nugget effect
(GNE) and the sampling nugget effect (SNE). Some deposits
naturally have an inherently high GNE, which can be inflated
through poor quality sampling.
A major cause of SNE is the heterogeneity of broken rock
(e.g. a rock pile, crushed rock or pulp), which to some extent
reflects the primary in situ heterogeneity. In this context, heterogeneity is defined as the nature of the lot, in which all the
contained fragments are non-identical. In this case, two types
of heterogeneity are defined: the constitution heterogeneity
(CH), and the distribution heterogeneity (DH). Constitution
heterogeneity and DH contribute to the SNE, through the FSE
and grouping and segregation (GSE) errors.
Throughout the mine value chain, optimised sampling
protocols aim to reduce the total sampling variance thereby
also reducing the total nugget variance; skewness of the data
distribution; and number of extreme data values.
Correct sampling errors

Correct sampling errors are considered correct because
they cannot be removed by correct sampling (Table 1; FSE
and GSE). They relate to the inherent heterogeneity of the
material being sampled and control sample precision (Pitard
1993).
Precision specifically relates to the CH of the material
in question and leads to the FSE. Poor precision in samples
generates ore/waste misclassification. The FSE can be estimated via the FSE equation (Franois-Bongaron and Gy
2002; Gy 1982). Out of all sampling errors, the FSE does
not cancel out and remains even after a sampling operation is
perfect. It is controlled via the optimisation of sample mass
and size reduction process (Petersen, Dahl and Esbensen
2004).
The DH and related GSE also contribute to sample precision. Distribution heterogeneity represents the difference
in average composition of the lot from one place to the next
in the lot; it is responsible for the irregular distribution of
grade and values in groups of fragments of broken ore.
The DH can be influenced by large differences in density
and fragment composition. Distribution heterogeneity of
a given lot is governed by CH, the spatial distribution of
fragments and the lot shape, thus leads to GSE. From a
practical perspective, GSE cannot be measured, but may
have a material effect on the total sample error (FranoisBongaron 2014; Pitard and Franois-Bongaron 2011). It
is controlled by accumulating many small increments to
form a composite sample. Segregation can theoretically be
reduced by homogenisation, though in the presence of liberated gold particles is a futile exercise that promotes further
segregation. The treatment of coarse-gold-bearing samples
is a special case (Dominy 2014a; Dominy and Petersen
2005; Royle 1989).
Table 1 Definition of sampling errors as defined in TOS (Gy 1982; Pitard 1993)
Sampling error
Acronym
Error type
Effect on sampling
Source of error
Error definition
Fundamental
FSE
Correct sampling
error (CSE)
Random errors
precision generator
Characteristics of
the ore type. relates
to constitution and
distribution heterogeneity
Grouping and
segregation
GSE
Delimitation
DE
Incorrect sampling
error (ISE)
Systematic errors
bias generator
Extraction
EE
Sampling equipment and materials

handling
Results from grade heterogeneity

of the broken lot. Of all sampling
errors, the FSE does not cancel
out and remains even after a sampling operation is perfect. Experience shows that the nugget effect
can be artificially high because
sample weights are not optimal
Relates to the error due to the
combination of grouping and
segregation of rock fragments in
the lot. Once rock is broken, there
will be segregation of particles at
any scale (e.g. surface stockpile
or laboratory pulp)
Results from an incorrect shape
of the volume delimiting a sample
Weighting
WE
Preparation
PE
Analytical
AE
Incorrect sampling errors

The incorrect sampling errors (ISE) (Table 1; DE to PE)
arise as a consequence of the physical interaction between
the material being sampled and the technology employed to
extract the sample. They result in bias, which can be reduced
by the correct application of sampling methods, equipment
and procedures (Esbensen and Paasch-Mortensen 2010; Gy
1982; Holmes 2015; Petersen et al. 2004; Pitard 1993, 2009).
The AE is generally not considered as an ISE, though
remains a potential bias generator. It can be minimised
through proper QAQC in the laboratory across staff activity,
and analytical equipment maintenance and calibration. It may
also be affected by rock matrix effects.
Defining a representative sample

A sample can be described as being representative when it
results in acceptable levels of bias and precision. The total
variance for resource and grade control sampling should not
be more than 32%, with the total FSE component not more
than 16% (Pitard 2013). The FSE is reported at a given
confidence limit, usually 68% or one standard deviation. All
sampling variances are cumulative and contribute to the total,
which in turn contributes to the SNE. In reality, FSE and GSE
Analytical process
Results from the incorrect extraction of a sample. Extraction is only

correct when all fragments within
the delimited volume are taken
into the sample
Relates to collecting samples
that are of a comparable support.
Samples should represent a
consistent mass per unit
Refers to issues during sample
transport and storage (e.g. mixup, damage, loss and alteration),
preparation (contamination and/or
losses), and intentional (sabotage
and salting) and unintentional
(careless actions and non-adherence of protocols) human error
Relates to all errors during the
assay and analytical process,
including issues related to rock
matrix effects, human error, and
analytical machine maintenance
and calibration
are likely to contribute up to 90%, with DE, extraction error

(EE) and AE up to 25% of the total (Pitard 1993).
FSE equation and application to gold ores

The FSE can be theoretically estimated before material is
sampled, provided characteristics (e.g. sampling constant
K) embedded in the FSE equation are determined (Gy 1982;
Pitard 1993). The equation addresses key questions of sampling broken rock:
what weight of sample should be taken from a larger
mass, so that the FSE will not exceed a specified
variance;
what is the possible FSE when a sample of a given
weight is obtained from a larger lot; and
before a sample of given weight is drawn from a larger
lot, what is the degree of crushing or grinding required
to lower error to a specified FSE. A technical issue with
the use of the FSE equation is the numerical value of
the power in the so-called liberation factor (FranoisBongaron 1998; Gy 2004). The problem was addressed
by Franois-Bongaron (1998), who suggested a modified FSE equation that includes the parameters and
liberation diameter (d) (Franois-Bongaron 1998;
Franois-Bongaron and Gy 2002).
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K can be experimentally determined using a sampling treebased method, which also yields a value for (FranoisBongaron and Gy 2002; Minnitt and Assibey-Bonsu 2010;
Minnitt, Rice and Spangenbeg 2007). In addition, the heterogeneity test (HT) can also be used to determine K, though
no value of is defined (Franois-Bongaron 1993; Pitard
1993; Magri 2007; Minnitt and Assibey-Bonsu 2010). The HT
possesses representivity challenges when applied to coarse
gold-bearing deposits (Dominy and Xie 2016).
As originally defined, d represents the mineral liberation
size below which 95% of the material must be ground in order
to liberate at least 85% of the gold (Gy 1982; Pitard 2004).
For gold mineralisation, d can be redefined to dm, representing the screen size that retains 5% of gold given a theoretical lot of liberated gold (Bazin, Hodouin and Blondin 2013;
Dominy 2014a; Franois-Bongaron and Gy 2002; Pitard
2015; Royle 1991). If coarse gold is dominant, then dm can
represent the coarse most influential population (Dominy et
al. 2012; Pitard 2009). If gold particles cluster, then dm should
be redefined as dclus (Dominy and Platten 2007; Pitard 2007,
2009). The value of K is dependent on the microscopic properties of the minerals, and varies with gold grade and dm or d.
A direct approach to the determination of gold particle
size and dm is suggested by some practitioners (Dominy et al.
2011; Dominy and Xie 2016; Pitard 2015). This may include a
combination of mineral particle size determination via optical
and/or electron/X-ray microscopy (Dominy et al. 2012; Lyman
and Schouwstra 2011) and/or crush-screen-concentration
(Dominy et al. 2011; Gonzales and Cossio 2007). Research
has indicated that can generally be taken as 1.5 (FranoisBongaron 1998; Franois-Bongaron and Gy 2002).
Gold mineralisation and sampling

Nature of mineralisation
Gold mineralisation frequently displays evidence of two populations, representing fine- and coarse-gold (above 100m)
particles (Dominy, Xie and Platten 2008; Dominy and Platten
2007; Pitard 2009). These may be a part of separate paragenetic stages. In general, the fine-gold particles are likely to
be relatively disseminated through the mineralisation and
responsible for a background grade of between 0.5 and 5g/t
Au (Dominy et al. 2008); whereas, coarse particles are likely
to be more dispersed and/or locally clustered, being critical
to economic viability in low-grade deposits.
Mineralisation containing substantive quantities of coarse
gold (>15% >100m) is often typified by a high-nugget effect,
which represents variations in: (1) the in situ size distribution
of gold particles (including effects of gold particle clustering),
and (2) gold particle abundance (Dominy 2014a). Grade is
generally correlated to gold particle size, although the relationships are complex (Dominy and Platten 2007; Dominy
et al. 2008). Higher grades often relate to abundant coarsegold and/or clustered gold particles. The coarse-gold particle
population will generally be challenging to sample compared
to the fine-gold population (Dominy 2014a).
Peculiarities of gold sampling

There are a number of peculiarities of sampling for gold,
which relate to both CSE and ISE. Those that drive FSE
include:
primary gold particle distribution is often erratic (high
GNE), with localised clustering effects (Dominy and
Platten 2007; Platten and Dominy 2003) and
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grades are relatively low (gram per tonne Au), thus gold
particles can be relatively rare events (e.g. Poisson
distribution) particularly in low-grade ores (Pitard and
Lyman 2013).
The gold content of a sample and the gold content
of the surrounding ore can be very different. Similarly,
there may be large differences between the primary
sample and subsequent sub-samples unless rigorous
optimisation is undertaken.
Those issues that contribute to the GSE and ISE include:
poor disintegration of gold particles during pulverising often lead to smearing and/or the coating of sample
preparation or testing equipment leading to PE (Dominy
and Petersen 2005; Pitard 2009)
high contrast between the densities of gold and gangue
minerals promote segregation once liberated, which
leads to GSE (Franois-Bongaron 2015; Pitard 2009)
and
bias during diamond drilling relates to the plucking of
gold particles from the core surface as a result of the
drilling process (Dominy 2014a; Pitard 2009), which
leads to a negative grade bias (EE). Core sawing can
also lead to gold loss in the cuttings (PE).
These problems can be overcome through the use of
larger sample and assay charges, and careful procedures
to minimise sampling errors.
Case studies
Introduction
The following case studies documented between 2001 and

2007 show sampling issues that can be found in gold projects
globally. Each case study is reported anonymously, and the
sampling errors and relative impact on the project are discussed. It was concluded that for all presented case studies,
the sampling issues were the most material. For those that
were producing operations, the resource/reserve estimation
process was considered appropriate.
Case study 1: Core quality issues

A shear-zone style deposit located in the Former Soviet Union
was at an advanced stage of evaluation as a joint open pit
and underground operation. A feasibility study had been
completed.
The deposit was characterised by steeply dipping goldquartz-sulphide veins up to 0.3m in width, forming a larger
1530m wide stockwork zone. The global reserve grade was
5.7gt1 Au. There was minimal coarse gold present, though
the deposit was nuggety due to the pod-like nature of the
sulphide mineralisation within the veins. The resource had
been diamond drilled on a relatively fine grid and had some
underground development in it. An estimate by the owner
defined Measured, Indicated and Inferred Mineral Resources
in accordance with the 2004 JORC Code.
During an independent review, it was found that there was
poor documentation with regard to QAQC and that the (total)
core recovery was generally between 44 and 71% with a mean
of 61%. The owner had drilled a number of confirmatory
diamond holes, whose recovery improved, but were still relatively low between 65 and 83%.
The low recoveries indicated that there was a large amount
of core (sample) loss, and that the actual sample collection
process was prone to a high EE. Further investigation showed
that core loss was principally related to the sheared and altered
nature of much of the mineralisation and to some extent drilling quality. The remaining half core was highly fragmented
and friable, testifying to the difficulty in cutting the original
sample. Where such a core problem exists, it is strongly recommended that after detailed logging and photography, the
entire core composite be crushed and then split for laboratory submission (Annels and Dominy 2003). A mineralogical
and assay investigation should be undertaken to ascertain the
impact of the core loss on the mineralisation.
These issues were of obvious concern and as a result,
the Measured blocks were reallocated to the Indicated and
Inferred categories, and Indicated Resources to the Inferred
category. Some previously Inferred blocks became unclassified. As a result of the resource downgrade, the company was
unable to raise the finance required for project development.
They had to fund additional diamond drilling to confirm their
expectations of the deposit, revise the feasibility study, and
undertake an investor relation programme to avoid loss of
confidence in the project.
Proper consideration of core quality early on would have
saved the operator both money and reputation. The additional
drilling used a triple tube core barrel and driller with improved
expertise in poor ground. In zones of poor core recovery, the
entire sample was crushed, split in half and one-half submitted
to the laboratory.
Case study 2: Incorrect compositing

The deposit was located in North America, where a new vein
system had been located between two former underground
operations. A steeply-dipping 3m to 5m wide vein had been
defined using diamond drilling on a 20m by 20m grid. All
drill cores were logged and 1m half-core lengths submitted
for 1-kg SFA. Coarse, often visible gold was known from the
previously mined veins and was confirmed in the new vein
by core logging and SFA.
A resource estimate yielded a global grade of 6.5gt1 Au,
which was lower than the expected 1015gt1 Au required
to support a small underground mine. The project was put
on hold.
A later review found that in the drive to collect 1m core
samples, any core samples on the footwall of the vein that
were <0.5m were bagged and not sent for assay. Geological
studies revealed that the footwall of the structure contained
a discrete high-grade vein bearing visible gold. This entire
mineralisation stage had been virtually excluded from the
estimate with a loss of 5060% of the gold inventory.
The remaining footwall (half) core was collected, assayed
by SFA and the resource re-estimated. The new global grade
was 12.9gt1 Au, much closer to expectation.
This example shows the clear need for proper training
of staff and communication between all parties. The project
geologists were focused with fixed core lengths, with no consideration that a geologically based sample regime was more
appropriate. In essence, this was an EE, where the mineralised
zone was not sampled fully. From a project perspective, this
error led a good project to be put on hold for 9months. The
project subsequently went into production, yielding a ROM
grade of 14gt1 Au over 4.5years.
Case study 3: What coarse gold?

A pseudo-coarse gold problem may be present in some gold
deposits, due to the presence of gold particle clusters that
give the effect of individual coarse-gold particles (Dominy
and Platten 2007). These clusters, which may be distributed

on the centimetre-scale or greater, give rise to high assay
variability in field samples. However, once a sub-sample is
pulverised, the effect of the clusters is removed if the individual gold particles making up the clusters are liberated. Thus,
any resulting pulp will tend to have lower variability, unless
true coarse-gold particles exist.
An Australian greenstone-hosted vein deposit was found
to have a coarse-gold problem. The vein had a mean width of
2.5m and a global reserve grade of 11gt1 Au. High variability
was found for the first 12months of reconciliation, where the
annual ROM grade was 7.5gt1 Au.
Checks of diamond half (NQ) core and laboratory pulp
duplicates indicated a very high variability, where 90% of the
data were 60% (half absolute relative difference: HARD) or
worse. The issue had been ignored, as there was apparently
no indication of visible gold within drill core. Assays were
based on a 30-g sub-sample for fire assay (FA) scooped from
the pulveriser bowl.
An initial review of metallurgical data indicated that a
gravity recoverable gold (GRG) yield of 55% was achievable,
suggesting that coarse gold was present. A number of samples
were taken from low- to high-grade intersections, where mineralogical studies revealed the presence of gold particles up
to 1mm in size, with many in the 150500m range.
A series of 50 half-core samples were taken for whole-sample SFA and it was found that between 15 and 75% of the gold
in the samples reported to the screen (mean 40%). A comparison was made between the new SFA grades and the original
30g FA, and it was found that the SFA were generally higher
than the original FA by about 20%.
Drill holes were re-logged and it was found that visible
gold was common. In addition, it was found that clusters
of visible gold particles extended over 2cm. This clustering resulted in increased heterogeneity within both half and
crushed core.
In this case, there was adequate QA, but no QC follow-up
since the pulp duplicate data were ignored. An inappropriate
sampling protocol in a clustered-coarse-gold environment
resulted in a high FSE. Furthermore, the pulps were prone
to a high GSE, as not all the coarse gold was reduced in size
during pulverisation. Scooping from the bowl was in effect
grab sampling with an inherent high DE and EE. Given the
presence of coarse gold, there was also the potential for contamination (PE) and the need for cleaning the pulveriser bowl
with a barren flush between samples.
Timely identification of visible gold in core should have
been achieved and acted upon. The original sample protocol was replaced by a half-core LeachWELL and effective
QC follow-up. Reconciliation improved over the following
6months, with grade and tonnes within 11% of expectation.
Case study 4: Gold segregation in pulps

An underground vein operation in North America was known
to contain coarse-gold particles up to 1.2mm in size, and
rarely up to 4mm. The plant recovered between 40 and 60%
of gold via a gravity circuit. The vein had an average width
of 2.5m and a global reserve grade of 17.8gt1 Au. Monthly
reconciliations were up to 50% on grade and up to 15%
on tonnes.
From drill core and underground chip samples, a 2-kg sample was pulverised and a 30-g FA undertaken. There was no
formal sampling protocol or laboratory QAQC system. With
new owners, systems were introduced into the pre-existing
133
laboratory. It was identified that the pulp duplicates displayed a very poor precision; where 90% of the data were
55% HARD. In addition, the pulverisers were not cleaned
between samples and there was evidence of gold contamination between some samples.
A number of exhaustive tests were undertaken on 2kg pulp
lots, where the pile was mixed, flattened and 40 consecutive
50g sub-samples taken for FA. The variability was very high,
and in one instance, the range between the minimum and
maximum values was 250gt1 Au.
These findings confirmed that the pulps were heterogeneous due to the poor comminution of gold particles during pulverisation and the excessive GSE within the pulps.
Different pulp sub-sampling techniques further augmented
the level of GSE. One laboratory technician homogenised
the pulp by mat rolling then simply scooped off 30g from
the top of the pile, thereby missing gold that had segregated
to the bottom of the pile. Another technician placed the pulp
on the mat, shook it rigorously, flattened the pile and cut a
series of sample lines through the pile with a greater chance
of picking up segregated gold at the pile base.
An additional issue of sample contamination was identified. Where very high-grade samples (>30gt1 Au) usually
bearing visible gold were present, the following sample or
two samples were often contaminated. Tests were undertaken,
where it was found up to 10% of the high grade was smeared
into the following samples. At the time, no barren flushes were
undertaken in the laboratory and equipment hygiene was poor.
In essence, the mat roll method understated, while the
shake, flatten and cut technique overstated the gold grade.
The recent mine records were revisited and it was found that
during a leave of absence by the overstating technician, a
number of stope blocks had been abandoned due to the low
sample grades achieved. The stope-bounding drives and raises
were subsequently re-sampled and assayed using the new
protocol. They were found to be of ore grade and were subsequently mined out recovering 11000oz Au.
The key issue was that coarse gold needs to be treated
differently. Pulps-bearing liberated gold cannot be homogenised; GSE can be highly problematic; and proper protocols
and procedures must be set up both in the mine and laboratory. An SFA was introduced to account for coarse gold,
along with improved laboratory procedures and staff training.
Full QAQC protocols were introduced, particularly covering
equipment cleaning and contamination monitoring. Barren
flushes between samples were introduced and were assayed
at a rate of 1 in 20. Where visible gold was observed or high
grades expected, additional barren samples were introduced
and subjected to FA.
Case study 5: Grab sampling for grade control

Grab sampling has been used as a grade control tool in
many gold operations globally (Dominy 2010). A shearzone hosted underground operation in Australia consistently
had reconciliation problems. Mineralisation did bear some
coarse gold, though this was not dominant. Most gold was
sulphide-hosted and below 150m in size. This was manifested as a general under-call with respect to the reserve
grade (7.4gt1 Au) of around 25%. The decision to send
material from the stockpile to the plant was based solely
on grab sampling.
Each stock pile represented approximately 500t of supposed ore. Twenty 3kg samples were taken from around
the edge of the stockpile, at a fragment size of generally
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<12cm. Each sample was sent to the laboratory for a 500g

LeachWELL-based pulverise-and-leach (PAL) assay.
A test study was undertaken based on 200 3-kg grab samples collected from a chosen stockpile. For the total population, the mean grade was 12.8gt1 Au, the minimum grade
0.01gt1 Au and the maximum grade 79.7gt1 Au. There are
a number of grade permutations possible if an exhaustive
20 set sample batches are drawn. Out of 200 samples, the
lowest grade combination of 20 samples was 0.1gt1 Au,
and the highest grade combination 49.1gt1 Au. The mean
was 10.6gt1 Au. The test stockpile was fed to the plant and
autosampler after secondary crushing, where a batch mean
head grade of 4.2gt1 Au determined. The mean of the first
20 samples taken was 8.2gt1 Au, which implies under normal circumstances that the lot would have been sent to the
plant as ore. At the time, a mine cutoff grade of 4.6gt1 Au
was applied.
The operation was battling reconciliation problems and
achieving a lower head grade. The reserve model was based
on diamond drill data on a 2030m by 2030m pattern. Face
chip sample data were ignored, as it was considered to be
biased and only represented around 50% of mine faces due
to operational constraints. As a result, all material dumped
on the surface stockpiles, which included mineralised waste,
and marginal, medium and high-grade ore, was grab sampled
prior to being sent to the waste tip or plant. Given the biased
nature of grab sampling, most of the mineralised waste and
marginal ore were sent to the plant diluting the ore feed. Grab
sampling was considered the key issue. The grade estimate
was also considered to be suboptimal.
This study showed that the use of grab samples to assess
grade is problematic. The majority of stockpiles were sent to
the mill as ore. This was in part related to a higher proportion
of gold in the fine (<1cm) fraction, thus biasing grab samples
high. An important point to note is that each grab sample or
group of 20 grab samples did not represent the stockpile. Grab
sampling is prone to chronic FSE, GSE, DE and EE (Dominy
2010; Pitard 2009). Fundamental sampling error calculations
indicated that a 25-t sample was required from the stockpile
to achieve an acceptable level of FSE.
Grade control subsequently re-focused to use the diamond drilling, which was closed to a 15m by 15m spacing.
LeachWELL (12kg) was used for all samples and grab sampling was stopped. The resource model was also improved
via the use of an optimised kriged block model. A managed
low-grade stockpile was introduced. Reconciliation improved
to 12% for grade and tonnes in 6 months.
Case study 6: Reverse circulation and blast

hole sampling
In many open pit gold projects, blast hole (BH) drilling has
been used as the principal grade control sampling method.
More recently, BH has been replaced with reverse circulation
(RC) drilling in an attempt to improve sample quality and
grade control outputs (Pitard 2008; Chieregati, El Hajj, Imoto
and Pignatari 2015).
This case study is based on an African open pit gold operation, working for a large tonnage low-grade (1.9gt1 Au)
greenstone-hosted shear-zone type deposit. Gold was principally distributed in quartz veins, though some local wallrock
disseminations were observed. The gold was quartz and/or
pyrite hosted, with minimal visible gold. About 20% of the
gold was gravity recoverable and mineralogical studies identified a maximum gold particle size of around 350m.
During the first few years of operation, all grade control

was undertaken as part of the BH drilling pattern, and samples were taken from the cuttings. Such a methodology is
known to be problematic with issues relating to DE, EE and
GSE, namely, hole-wall caving, sample loss into cavities,
contamination and particle segregation within the drill hole.
Delimitation error also existed where the hole was drilled
below the current bench the so-called sub-drill. In addition,
the collection of sample material from the surface cone was
fraught with problems relating to high FSE, pile segregation
(GSE) and sample delimitation and extraction (DE and EE).
In this case, BH samples were collected with a sectorial
or pie tray (approx. 10kg from 200kg, representing 2.5m),
providing an acceptable DE in some cases, though the EE can
be high due to overfilling resulting in sample loss. However,
half of the 10kg sample (e.g. 5kg) was poured (no splitter
used) into a bag for laboratory submission. After crushing
to P80 2mm, a 1kg sub-sample was taken and pulverised to
P90 75m and a 200g sub-sample riffle split and a 30g FA
undertaken. This protocol yielded an FSE of 92%.
Subsequently, RC drilling with a face hammer bit was
introduced for grade control. Reverse circulation has many
improvements over BH drilling through the air propelled
recovery of the drill chippings up the centre of the drill rod,
which leads to a reduction in contamination and improved
mass recoveries. It also provides improvements in grade and
geological resolution (a closer spacing than BH and capability for angled holes to reflect the mineralisation trend) and
reduced overall sampling error (reduced FSE, EE, DE and
GSE). The key issue with taking a sub-sample from a 200kg
lot of chippings is that the FSE can only be lowered by either
reducing the entire nominal fragment size of the entire lot or
by taking a bigger sample. The RC drilling produced a finer
product and the run length was reduced to 0.7m to decrease
the primary sample size. A 10kg RC sample was collected via
a cone splitter at the rig. At the laboratory, this was crushed to
P80 1.5mm, 5kg riffle split for pulverisation, and 1kg taken
for a LeachWELL assay. The overall FSE for this protocol
was 29%, a clear improvement over the old BH protocol.
This was still not an optimal figure, but an overall improvement was achieved. At the time of introduction, it was possible to compare the drilling and assay results of both the BH
and RC samples for a number of benches. It was found that the
RC drilling protocol yielded a nugget effect of 44%, whereas
the BH samples gave a value of 62%.
An improvement supporting the use of RC versus BH drilling for grade control was seen. However, a level of compromise
had to be accepted, even with the sampling protocols for RC
where a large field sample can be required to minimise the FSE.
Case study 7: Uncertainty in heterogeneity

testing in coarse-gold ores
The HT is a common approach to determine the value of K for
FSE equation use. The method consists of extracting a number
of fragments at random from different size fractions of the lot.
The number of individual fragments should generally be as

large as possible, but for practical purposes is suggested to be
around 50 (Gy 1982; Franois-Bongaron 1993; Pitard 1993).
Table 2 shows variability in HT results from North
American coarse-gold-bearing mineralisation. The mine operator aimed to optimise sampling protocols and undertook a
HT on ore fragments from a stockpile. The initial test (Test
#01 in Table 2) yielded a relatively low K value. Sampling
protocols were optimised for this figure.
A later review noted that the K value was below expectation given that the mine recovered some 65% of its gold
via gravity and that visible gold was common in both drill
core and underground exposure. Three additional tests were
undertaken, this time with 100 fragments in each test lot (Tests
#02-04; Table 2). The K values defined displayed strong variability ranging from 230 to 2600gcm1.5. Test #04 yielded
a particularly high value for both K and d, being related to
two very high grades. A fifth test was undertaken using 200
fragments of 1kg weight.
A study was undertaken of gold particle size and distribution based upon mineralogical observation, inspection of
gravity concentrates and metallurgical screening and assay
tests. It concluded that for ROM grade ore of 15gt1 Au, the
d value was 3mm.
The original sample protocol was based on half HQ core
sampling, pulverising of the entire sample, and sub-sampling
500g for a later sub-sample of 30g for FA. Duplicate pulp FA
were rarely undertaken, but those undertaken showed high
variability (90% within 70% HARD). Test work also identified coarse-gold contamination between samples preceded
by high-grade material. Two barren flushes were introduced
after any sample-bearing visible gold or expected to be high
grade. Protocols were adjusted to take into account the coarse
nature of mineralisation through the total SFA of all half core
or face samples.
In many cases where coarse-gold particles are relatively
sparsely distributed, the picking of 100 test fragments is likely
to only represent low-grade fine-gold background population
(Dominy 2014a). This example shows that the calibration of
the FSE equation using HT can be problematic in the coarsegold environment (Dominy and Xie 2016). It is generally
found that a direct approach to ddetermination is more
appropriate (Dominy et al. 2011; Pitard 2015).
Case study 8: Case of QA with no QC

A greenstone-hosted disseminated gold deposit in Central
Africa had been drilled out by three NQ diamond drill campaigns. Spatially, the three sets of drilling broadly covered the
same mineralised zones. The gold is fine-grained, hosted in
pyrite and/or arsenopyrite and generally below 50m in size.
The largest campaign contained 60% of the assay database
that was used for resource estimation.
During an independent review of the resource, it was found
that the key drill programme had problematic QAQC data. In
particular, the results for the CRMs, inserted at a rate of about
Table 2 Fifty, 100 and 200 piece experiments for a coarse-gold ore deposit in North America. All fragments were approximately
1.5kg (equivalent particle size diameter 16cm) and where pulverised in their entirety and subsequently screen fire assayed
Test no.
01
02
03
04
05
No of test fragments
Grade of lot (gt1 Au)
K value (gcm1.5)
Calculated liberation diameter (m)
50
100
100
100
200
3
7
16
270
46
180
230
290
2600
1300
40
90
160
4300
900
135
1 in 30, were consistently high. The results of inter-laboratory check pulp samples, submitted at a rate of 1 in 50 were
overall biased low.
The sample collection and preparation protocols were
found to be acceptable. Despite the high bias indications of the
CRM data, the implications were ignored in the resource estimate. Detailed review showed that the entire batch of assays
was about 36% higher with respect to grade. This error was
shown to relate to the laboratory, where poor maintenance
and calibration of AAS equipment led to high AE. This is an
example of clear QA with no supporting QC.
The remaining half core was assayed using the same protocol at a different laboratory. CRMs were inserted at a rate
of 1 in 20. The resource was re-estimated, which led to the
deposit grade reducing from 1.8 to 1.5gt1 Au. This resulted
in project suspension and withdrawal of funding.
Case study 9: Poor mill balance sampling

An underground operation in South America was extracting 100000t per annum at 15gt1 Au. Much of the gold was
coarse (up to 2mm in size), with the processing plant based
on a 13th1 gravity-only circuit to extract around 8085% of
the gold. On an annual basis, the operation was expected to
produce around 40000oz Au. By the end of the first year of
production, the operation had produced 31000oz Au. Based
on the mill balance, a recovery of 94% was calculated from a
head grade of 10.3gt1 Au and mean tailings grade of 0.6gt1
Au.
A review of all aspects of grade control and reconciliation was undertaken. It was found that the tailings grades
were based on a single 1kg hand sample collected via a small
bucket once per hour, and this was sometimes missed. Thus
13t of ore was represented by a 1kg tailings sample. A series
of 250kg bulk samples of tails were collected and tested in
a metallurgical laboratory. It was found that the grade of
these averaged around 2.5gt1 Au and that gold particles up
to 0.75mm were contained. An autosampler was fitted to the
tails outflow, which was initially set to collect a 2.5kg sample
every 5min. Over a period of 1month, this revealed grades
averaging 3gt1 Au and on a shift basis up to 6.5gt1 Au. These
high grades were linked back to the gravity circuit, which was
not optimised and thus coarse gold was being lost.
The initial tailings sample yielded an FSE of 51%,
together with increased DE and EE using a manual sampler.
The revised test protocol dropped the FSE to 9% and importantly took multiple increments over an hour thus having a
higher probability of collecting a coarse-gold particle(s). By
collecting multiple samples, the periodic fluctuation error was
also reduced (Pitard 1993). An autosampler was also introduced. In the original protocol, the small hourly samples did
not resolve periodic pulses of gold lost to the tails stream,
which represented higher feed grades to the gravity circuit.
The incorrect tails sampling was understating the actual gold
content by 6700oz, which was effectively unaccounted for in
the mill balance and hence a high recovery was calculated.
The study led to a number of changes in the plant to
improve recovery, including modifications to the grinding
circuit to grind finer and improvements to the gravity circuit.
The post-modification tailings sample protocol was reduced to
1kg sample per 20min, which given the removal of the coarse
gold yielded an FSE of 7%. Six months after modifications,
plant recovery had increased to 89%, based on a 13.5gt1 Au
head grade.
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Case study 10: Poor metallurgical sampling

strategy
A South American project was being evaluated with the intent
to re-commence underground operations. Mineralisation is
dominated by quartz-sulphide reefs generally 1m in width
hosted in granodiorite. Economic grades are related to ore
shoots, which extended around 75m along strike and >300m
down plunge. The central 25m core of the Main Reef ore shoot
contains a high-grade zone at 1530gt1 Au, compared to the
48gt1 Au in peripheral zones. Gold mineralisation contained
coarse gold up to 2.5mm in size, particularly in the core zone.
Finer gold (<0.15mm) was common in the peripheral zones.
Historical mining had previously used simple gravity and
amalgamation methods to extract gold, yielding recovered
head grades in the 1525gt1 Au range. As part of the evaluation programme, HQ diamond core drilling was undertaken.
Core recovery and quality was good.
During re-evaluation, two 100kg diamond half-core composites (H#1 and H#2) were taken for metallurgical recovery
testing based on the standard GRG test. The two samples
were crushed to P80 3mm and 25kg split off for GRG testing.
Composite head grades were 36 and 47gt1 Au for H#1 and
H#2 respectively, yielding GRG values of 90 and 96%. A single 100kg half-core composite was taken from the low-grade
peripheral zone (L#1), the sample was crushed to P80 3mm
and 25kg split off for GRG testing. This yielded a head grade
of 16gt1 Au and a GRG value of 81%.
Based on these results, a 75000t per annum gravity plant
was built, with a recovery expectation of 70%. The expected
head grades of 15gt1 Au were not being achieved, yielding
around 5gt1 Au and a gold recovery of 3040%.
A number of issues related to geological interpretation and
metallurgical sampling were identified. The original metallurgical samples H#1 and H#2 were from very high-grade core
mineralisation, and were not representative of that domain.
Only two samples were collected. Sample L#1 was unrepresentative of the low-grade zone, and was biased by one
intersection of relatively high-grade material that was present
in the low-grade zone. Only one sample was collected.
During sample preparation, the crushing and splitting of
the 100kg samples down to 25kg test masses yields a high
FSE (up to 38% at 90% confidence), where less than 15%
would be preferable. In addition, the splitting process after
crushing was based on shovelling 25kg directly into buckets from a pile. The splitting of metallurgical test sub-samples from a primary composite is a key issue, where the
split process is not representative (Dominy 2014b). This is
further compounded when the primary sample is not representative either. In this case, the sub-sampling process was
non-equiprobable with high risk of DE, EE and GSE.
Geological interpretation of the high-grade zone focused
on a continuous zone down the centre of the shoot (considered to be 35% of the shoot). This was not the case, where in
reality there was a high-grade core but it comprised a series
of en-echelon sub-shoots, which only accounted for about
15% of the shoot. The high-grade zone contains a high-level
of GRG, whereas the low-grade zones contain substantially
less. This lead to a reserve grade bias (15 versus 5gt1 Au)
and over-reliance on GRG gold for plant design.
Subsequent metallurgical testing of the low-grade shoot
indicated that an achievable GRG was in the range of 2025%
with most of the gold (>7080%) being sub-100m, sulphide-hosted and requiring 24h leaching to achieve a 7585%
recovery.
Table 3 Summary of case study conclusions. Sampling errors defined in Table 1

Case
Dominant sampling errors
Stage of sampling issue
Key sampling issues
1
2
EE and DE
EE
Core drilling and sampling

Core sampling
FSE, GSE, DE, EE and PE
Core sampling, sample preparation and assay method

Sample preparation and assay
method
FSE, GSE, DE and EE
AE
Analytical method
9
10
FSE, GSE, DE and EE

FSE, GSE, DE and EE
Sampling method
Sample selection strategy and
sample preparation
Core loss led to poor core sample quality. Poor QAQC

Poor geological understanding and compositing strategy
led to sections of drill core not being submitted for assay
Whole-sample pulping, pulp splitting and fire assay
inappropriate
Poor laboratory practice led to massive bias via inappropriate pulp splitting and fire assay inappropriate. No
QAQC
Grade control process over-reliant on grab sampling from
stockpiles, followed by fire assay
Grade control process over-reliant on reverse circulation
(RC) drilling, followed by fire assay
In the coarse-gold environment the application of the
heterogeneity tests often provide misleading results. Pulp
splitting and fire assay inappropriate
Poor AAS maintenance and calibration led to elevated
grades
Small samples taken at irregular intervals by hand
Original metallurgical samples taken from very high-grade
unrepresentative material. Primary samples were poorly
sub-sampled for testing
Sampling method, sample

preparation and assay method
Sampling method, sample
preparation and assay method
Sample preparation and assay
method
A further metallurgical testing programme for the lowgrade domain was instigated (25 75100kg samples), which
ultimately led to the commissioning of a CIL plant at the
mine. After further controls on mining were applied and the
operation of the new CIL circuit, head grades were increased
to 13gt1 Au, with recoveries between 90 and 95%.
Discussion
The sampling issues reported in the case studies relate to the
full range of TOS errors (Table 3), that resulted in monetary
and intangible losses (Table 4). These errors were reduced
through the implementation of new protocols, often supported
by new or additional ore characterisation (Table 5).
Quality assurance/quality control issues in Case 1 relate to
poor QA and lack of QC implementation. Accepted QAQC
procedures are well-documented and require appropriate

training and implementation (Abzalov 2008; DS3077 2013;
Sketchley 1998; Valle 1998). Full and timely analysis of QA
data is required and must lead to investigation if required.
Inappropriate sample type is exemplified in Cases 5 and
6, where grab samples are used for underground grade control and BHs for open pit grade control. Both methods have
well-documented issues, and their use is discredited in many
circumstances. Alternatives for underground grade control
include better use of geology and geological mapping, and
closer-spaced diamond drilling. For open pit grade control,
the application of RC drilling is recommended. Reverse circulation drilling has also been applied in the underground
environment with some success (Clark and Carswell 2014).
Inappropriate coarse-gold sampling protocols for resource
estimation and grade control led to problems in Cases 4 and
7. Protocols may involve pulverisation of an entire sample,
Table 4 Estimated monetary and intangible loss estimates for case studies. Monetary loss includes estimate of correction cost.
For operations, includes loss in revenue from poor reconcilation (i.e. gold loss from actual versus planned). Monetary
loss is on an annual basis for operations and over the delay period for development projects. For development projects
includes sustaining cost over delay period
Case study
Project status
Estimated US$
loss (M, million)
OD/UD
$34
UD
$23
UO
$810
UO
$810
UO
$23
OO
$23
UO
$34
OD
$34
UO
$56
10
UD
$23
Intangible loss
Project delay 18months. Company and management reputation.
Delays in capital investment
Project delay 9months. Company and management reputation. Delays
in capital investment
Management reputation. Fraught internal relationships. Time to implement improvements
Project delay 18months. Company and management reputation.
Delays in capital investment
Project delay 9months. Company and management reputation. Delays
in capital investment
Key: OD: open pit in development; UD: underground in development; OP: open pit in production; UP: underground in production.
137
Table 5 Summary of original and revised sampling protocols

Case study
Original sample protocol
Revised sample protocol
a) Half diamond core

b) Crush and pulverise all sample
c) Split 200g for 30g fire assay
Poor QAQC
a) Fixed 1m sample length

b) Total sample SFA
a) Diamond core and RC
b) Crush and pulverise entire sample
No QC
a) Half diamond core and face samples
d) Poor laboratory consistency on pulp splitting
a) Half diamond core (triple tube)

b) Crush to P80 2.5mm and riffle split 50%
c) Pulverise and riffle split 150g for 30g fire assay
For poor recovery zones, crush entire interval and riffle split half.
Implement full QAQC programme
a) Sample to geology
b) Total sample SFA
b) Crush and pulverise all sample
c) Total sample LeachWELL
Improved QAQC programme
c) Total screen fire assay
d) Removed need for pulp splitting. Implement full QAQC programme, including barren flushes between high-grade sample
No QAQC
a) Grab sampling, approx. 3kg (stockpiles)
b) Crush entire sample to P90 2mm
c) Riffle split 0.5kg for LeachWELL pulverise
and leach (PAL)
a) Blasthole (1m composites)

b) Split approx. 5kg from pile
c) Crush (P80 3mm) and pulverise entire
sample
d) Split 200g for 30g fire assay

Minimal AAS maintenance and incorrect calibration of AAS. Poor QC

a) Manually collected tails sample (1kg/h)
b) Pulverise and split for 30g fire assay
Poor sampling strategy
Splitting of 25kg test sample from 100kg
primary sample in low-grade ore
9
10

b) Samples crushed to P80 2mm and riffle split 50%
c) Total sample LeachWELL
Grab sampling ceased. Drill spacing reduced. Better use of geology
a) Reverse circulation (0.7m composites)
b) Split approx. 10kg at rig
c) Crush to P80 1.5mm and riffle split 1kg
d) Pulverise
e) Total sample LeachWELL
c) Total screen fire assay
Introduce barren flushes between high-grade sample
Full/regular AAS maintenance programme. Per shift calibration of
AAS, with mid-shift check. Improved QAQC programme
a) Tails autosampler (5kg/h)
b) Pulverise and split for 30g fire assay
Considered sampling strategy based on grade control sampling of
underground development along high-grade and low-grade zones.
Entire GRG samples tested (75100kg)
Table 6 Key stages in the design and implementation of a new or revised sampling protocol
Stage
Aim
Actions
Business case
Characterise
Design
Implement
Monitor
Update
Stakeholder engagement
Define aim(s) of protocol and set data quality objectives
Preliminary review and design of characterisation programme
Undertake characterisation programme
Review and interpret from Stage 2
Design sampling protocols within framework of theory of sampling (TOS)
Cost benefit analysis
Set-up systems and written codes of practice
Training of staff
On-going QAQC
Annual internal and/or external peer review of systems
Annual internal and/or external peer review of individuals
On-going training/re-fresher
Revision of protocols if deemed necessary in Stage 5 return to Stage 2 or 3 as appropriate
which results in gold liberation. In such a case, sample splitting is problematic other than with a rotary sample splitter.
Any homogenisation attempt will be useless and merely promote GSE. Mat mixing and scooping from a pile of pulp
should be avoided at all costs. A large sample assay method,
such as SFA or LeachWELL, is optimal. Good preparation
equipment hygiene is required. Barren flushes of the pulverising equipment should be undertaken between each sample.
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Poor core recovery (Case 1) typically reflects poor drilling

and/or ground conditions (Annels and Dominy 2003). Where
this is unavoidable, there will be a strong bias in assay grade
due to mineral loss. From a sampling perspective, the best
option is to either (a) assay the entire sample length or (b) to
crush it and split off a proportion for laboratory submission.
Poor laboratory practice in Cases 3 and 8 led to bias.
One case study (3) shows a common issue of handling pulps
containing liberated gold. Scooping from the pile in any

fashion will be affected by the segregation of liberated gold
particles. The incorrect calibration of analytical equipment
is careless.
An inappropriate sampling strategy for the plant balance
led to erroneous reconciliation in Case 9. The flawed protocol
was poorly executed. Manual samplers cannot be considered
as best practice. In addition, the protocol was not optimised
for the coarse-gold ore type.
Poor sampling strategy is shown in Cases 2 and 10, where
grade distribution and/or geology were ignored. Effective
understanding of the ore zone and likely geometallurgical
domains are critical to designing grade and metallurgical
sampling programmes.
Conclusions
(1)Sampling errors across the entire mine value chain
generate both monetary and intangible losses. At the
project development stage, these losses can relate to
biased resource/reserve estimates, potential project
delay and/or wasted/misused capital. During mine
operation, issues principally relate to ore/waste misclassification and poor reconciliation. In all cases,
there are monetary costs in correcting protocols.
Intangible costs relate to people and company reputation, poor relationships between technical disciplines, and wasted time enforcing poor protocols and
implementing new ones.
(2)In many cases, project teams are more interested in the
effects of poor sampling than dealing with the cause.
For example, during poor reconciliation, disciplines
often spend more time trying to apply correction factors and/or apportioning blame. Management and
practitioners often consider sampling to be of minimal importance, which reflects a lack of knowledge
and understanding of its proper application across the
mine value chain.
(3)Design of an optimised sampling protocol must consider its aim and objective (s) in context of ore type
and position in the mine value chain. In most cases,
a dedicated ore characterisation programme will be
required to support application of TOS and final protocol design. An approach to protocol design is presented in Table 6.
(4)The optimisation process should consider:
geological/mineralogical nature of ore type(s) and
likely geometallurgical domains and relationship to
grade. Characterisation with respect to gold particle
sizing, mineralogy and heterogeneity is critical
whole core sampling followed by full sample assay
via SFA or LeachWELL effectively yields FSE and
GSE values of zero. With good laboratory practice,
the PE and AE can be minimised. Arguments against
whole core sampling revolve around no reference
core remaining, though this author contends that
with modern digital photography and detailed logging, this should not be an issue
alternatively, RC drilling may be considered given
that it provides a larger field sample size than core,
though there is a loss of geological information and
extreme care must be taken during sample splitting
and assaying
application of TOS and FSE equation to optimise
protocols
avoiding gold liberation, except during pulverisation

of the final assay charge sub-sample and test for possible contamination in coarse-gold ores
using effective large assay charge techniques, such
as SFA or LeachWELL, if coarse gold is present; or
whole-sample processing via a laboratory-scale system
ensuring that separate splitters, crushers and pulverisers are used where coarse gold is present and that
equipment is effectively cleaned between samples
and blanks are used
in the plant, autosamplers taking multiple increments
should be used supported by appropriate sample
preparation and assay protocols

carrying out systematic QAQC programmes to
measure the reliability of each of the sampling,
preparation and assaying steps, and then optimising
the process and
proper documentation, staff training and periodic
review.
(5)Throughout any sampling and assaying or test work
programme, QAQC must be a primary feature.
Metallurgical sampling and test work programmes
frequently have minimal to zero QAQC. Protocols
must be set up with judicious consideration to cover
field collection and security, laboratory preparation
and analysis/testing to minimise sampling errors.
(6)The overall conclusion of this discourse is that correct sampling and assaying practices are critical to a
profitable gold mining industry. Management, technical and field staff should be educated to sample
better throughout the mine value chain. A project or
operation should appoint an appropriately trained TOS
champion to drive best practice. Good resources now
exist to service this need, both in the form of consultants and educators, and a new international sampling
standard (DS3077 2013). It is now time for TOS to
be integrated into international reporting codes (e.g.
JORC Code 2012).
Acknowledgements
The author would like to acknowledge the companies
who have consented to the presentation of the case studies
under confidentiality agreements. The late Dr Allen Royle
(University of Leeds, UK), Professor Yuling Xie (University
of Science and Technology Beijing, PRC), Professor Richard
Minnitt (University of Witwatersrand, RSA) and Professor
Kim Esbensen (GEUS, Denmark) are thanked for helpful discussions. Mining Technology reviewers are acknowledged for
their constructive comments on the manuscript.
References
Abzalov, M. Z. 2008. Quality control of assay data: a review of procedures
for measuring and monitoring precision and accuracy, Exploration and
Mining Geology, 17, 131144.
Afewu, K. I. and Lewis, G. O. 1998. Sampling a run-of-mine mill feed a
practical approach, Journal of the Southern African Institute of Mining
and Metallurgy, 98, 299304.
Annels, A. E. and Dominy, S. C. 2003. Core recovery and quality: important
factors in mineral resource estimation, Applied Earth Sciences Transactions
of the Institutions of Mining and Metallurgy, 112, 305311.
Bazin, C., Hodouin, D. and Blondin, R. M. 2013. Estimation of the variance
of the fundamental error associated to the sampling of low grade ores,
International Journal of Mineral Processing, 124, 117123.
Carrasco, P. C. 2009. Nugget effect artificial or natural?Proceedings of World
Conference on Sampling and Blending, 211217, Johannesburg, Southern
African Institute of Mining and Metallurgy.
139
Carrasco, P. C., Carrasco, P. and Jara, E. 2004. The economic impact of

incorrect sampling and analysis practices in the copper mining industry,
Chemometrics and Intelligent Laboratory Systems, 74, 209214.
Chieregati, A. C., El Hajj, T. M., Imoto, C. F. and Pignatari, L. E. C. 2015.
Validation of reverse circulation drilling rig for reconciliation purposes,
TOS Forum, 5, 105110.
Cintra, E. C., Scabora, J. A., Viegas, E. P., Barata, R. and Maia, G. F. 2007.
Coarse gold sampling at Sao Francisco mine, Brazil, in Proceedings of
World Conference on Sampling and Blending, 187197, Porto Alegro,
Fundacao Luiz Englert.
Clark, F. and Carswell, J. T. 2014. Using RC drilling to improve sampling in
a complex underground gold operation approach to underground grade
control at the Sunrise Dam mine, WA, in Proceedings of International
Mining Geology Conference, 143152, Melbourne, Australasian Institute
of Mining and Metallurgy.
Cossio, S., Noyola, J. -L., Gonzalez, P. and Espinosa, R. 2004. Sampling and
assaying of coarse gold at La Herradura, Mexico, CIM Bulletin, 1084, 15.
Dominy, S. C. 2010. Grab sampling for underground gold mine grade control,
Journal of the Southern African Institute of Mining and Metallurgy, 110,
(2010), 277287.
Dominy, S. C. and Petersen, J. S. 2005. Sampling coarse gold-bearing
mineralisation developing effective protocols and a case study from the
Nalunaq mine, southern Greenland, in Proceedings of World Conference
on Sampling and Blending, 151165, Melbourne, Australasian Institute
of Mining and Metallurgy.
Dominy, S. C. 2014a. Predicting the unpredictable evaluating highnugget effect gold deposits, in Mineral resource and ore reserve
estimation, 659678, Melbourne, Australasian Institute of Mining
and Metallurgy.
Dominy, S. C. 2014b. Effects of sample mass on gravity recoverable gold
test results in low grade ores, Applied Earth Sciences Transactions of the
Institutions of Mining and Metallurgy, 123, 234242.
Dominy, S. C. and Platten, I. M. 2007. Gold particle clustering a new
consideration in sampling applications, Applied Earth Sciences
Transactions of the Institutions of Mining and Metallurgy, 116, 130142.
Dominy, S. C. and Xie, Y. 2016. Optimising sampling protocols via the
heterogeneity test: challenges in coarse gold mineralisation, Mining
Technology Transactions of the Institutions of Mining and Metallurgy,
in press.
Dominy, S. C., Johansen, G. F., Annels, A. E. and Cuffley, B. W. 2000. General
considerations of sampling and assaying in a coarse gold environment,
Applied Earth Sciences Transactions of the Institutions of Mining and
Metallurgy, 109, 145167.
Dominy, S. C., Nopp, M. A. and Annels, A. E. 2004. Errors and uncertainty
in mineral resource and ore reserve estimation: the importance of getting
it right, Exploration and Mining Geology, 11, 7798.
Dominy, S. C., Platten, I. M., Howard, L. E., Bell, R-M., Xie, Y. and Minnitt,
R. C. A. 2012. Determination of the sampling liberation diameter in a highgrade coarse gold ore by high-resolution X-ray computed tomography, in
Proceedings of Sampling Conference, 161169, Melbourne, Australasian
Institute of Mining and Metallurgy.
Dominy, S. C., Platten, I. M., Xie, Y. and Minnitt, R. C. A. 2011. Underground
grade control protocol design: case study from the Liphichi gold project,
Larecaja, Bolivia, Applied Earth Sciences Transactions of the Institutions
of Mining and Metallurgy, 119, 205219.
Dominy, S. C., Xie, Y. and Platten, I. M. 2008. Gold particle characteristics
in narrow vein deposits: implications for evaluation and metallurgy, in
Proceedings of Narrow Vein Mining Conference, 91104, Melbourne,
Australasian Institute of Mining and Metallurgy.
DS3077. 2013. Representative sampling horizontal standard, Copenhagen,
Danish Standards Foundation.
Esbensen, K. H. and Paasch-Mortensen, P. 2010. Process sampling: theory of
sampling the missing link in process analytical technologies, in process
analytical technology. 3780, Chichester, Wiley.
Fallon, M., Rowley, M., Du Plessis, E., Golenya, F., Robertson, I. and
Swanson, R. 2012. Confirming the sampling, sample preparation and
assaying protocols used at two Yilgarn gold deposits, in Proceedings of
Sampling Conference, 4762, Melbourne, Australasian Institute of Mining
and Metallurgy.
Franois-Bongaron, D. M. 1993. The practice of the sampling theory of
broken ores, CIM Bulletin, 86, 7581.
Franois-Bongaron, D. M. 1998. Extensions to the demonstration of Gy's
formula, Exploration and Mining Geology, 7, 149154.
Franois-Bongaron, D. M. 2004. Theory of sampling and geostatistics: an
intimate link, Chemometrics and Intelligent Laboratory Systems, 74,
143148.
Franois-Bongaron, D. M. 2008. A brief history of Pierre Gy's sampling
theory and current trends in its acceptance in the mining world, in
Proceedings of Sampling Conference, 1314, Melbourne, Australasian
140
Mining Technology
2016VOL. 125NO. 3
Franois-Bongaron, D. M. 2014. State of affairs and current research trends

in theory of sampling fundamentals, including segregation and correctness,
in Proceedings of Sampling Conference, 1115, Melbourne, Australasian
Franois-Bongaron, D. M. 2015. Future challenges and research: theory of
sampling (TOS), TOS Forum, 3, 45.
Franois-Bongaron, D. M. and Gy, P. M. 2002. The most common error in
applying Gy's formula in the theory of mineral sampling and the history
of the liberation factor, Journal of the Southern African Institute of Mining
Geelhoed, B. 2011. Is Gy's formula for the fundamental sampling error
accurate?, Experimental evidence, Minerals Engineering, 24, 169173.
Giblett, A., Dunne, R. and McCaffery, K. 2012. Defining practical metallurgical
accounting discrepancy limits for gold operations, in Proceedings of Mill
Operators Conference, 39, Melbourne, Australasian Institute of Mining
and Metallurgy.
Gonzales, P. and Cossio, S. 2007. A review of sampling protocol for a gold
ore based on liberation study, in Proceedings of World Conference on
Sampling and Blending, 163174, Porto Alegre, Fundacao Luiz Englert.
Guresin, N., Lorenzen, L., Dominy, S. C., Muller, H. and Cooper, A. 2012.
Importance of effective sampling and test work protocols for process plant
design, in Proceedings of Sampling Conference, 95107, Melbourne,
Gy, P. M. 1982. Sampling of particulate materials, Amsterdam, Elsevier.
Gy, P. M. 2004. Sampling of discrete minerals a new introduction to the
theory of sampling I: qualitative approach, Chemometrics and Intelligent
Laboratory Systems, 74, 724.
Holmes, R. J. 2004. Correct sampling and measurement the foundation
of metallurgical accounting, Chemometrics and Intelligent Laboratory
Systems, 74, 7183.
Holmes, R. J. 2015. Sample station design and operation, TOS Forum, 5,
119128.
JORC. 2012. Australasian code for reporting of exploration results, mineral
resources and ore reserves, the JORC code. Joint Ore Reserves Committee
of the Australasian Institute of Mining and Metallurgy, Australian Institute
of Geoscientists and Minerals Council of Australia.
Lyman, G. J. and Schouwstra, R. 2011. Use of scanning electron microscope
to determine the sampling constant and liberation factor for fine materials,
in Proceedings of World Conference on Sampling and Blending, 89103,
Santiago, Gecamin.
Magri, E. J. 2007. Some experiences in heterogeneity tests and mine sampling,
Porto Alegre, Fundacao Luiz Englert.
Minnitt, R. C. A. 2007. Sampling: the impact on costs and decision making,
Journal of the Southern African Institute of Mining and Metallurgy, 107,
451462.
Minnitt, R. C. A. 2013. Sampling in the South African minerals industry, in
Proceedings of Sampling and Analysis Conference, 128, Johannesburg,
Southern African Institute of Mining and Metallurgy.
Minnitt, R. C. A. and Assibey-Bonsu, W. 2010. A comparison between
the duplicate series method and the heterogeneity test as methods for
calculating the sampling constants, Journal of the Southern African
Institute of Mining and Metallurgy, 110, 251268.
Minnitt, R. C. A., Rice, P. M. and Spangenbeg, C. 2007. Part 2: experimental
calibration of sampling parameters K and alpha for Gy's formula by the
sampling tree method, Journal of the Southern African Institute of Mining
Morrison, R. and Powell, M. 2006. Design for sampling preliminary
exploration, Journal of the Southern African Institute of Mining and
Metallurgy, 106, 697706.
Petersen, L., Dahl, C. K. and Esbensen, K. H. 2004. Representative mass
reduction in sampling a critical survey of techniques and hardware,
Chemometrics and Intelligent Laboratory Systems, 74, 95114.
Pitard, F. F. 1993. Pierre Gy's sampling theory and sampling practice, Boca
Raton, CRC Press.
Pitard, F. F. 2004. Effects of residual variances on the estimation of the
variance of the fundamental error, Chemometrics and Intelligent
Laboratory Systems, 74, 149164.
Pitard, F. F. 2007. The in-situ nugget effect: a major component of the random
term of a variogram, in Proceedings of World Conference on Sampling and
Blending, 91110, Porto Alegre, Fundacao Luiz Englert.
Pitard, F. F. 2008. Blasthole sampling for grade control the many problems
and solutions, in Proceedings of Sampling Conference, 1521, Melbourne,
Pitard, F. F. 2009. Pierre Gy's theory of sampling and C.O. ingamells poisson
process approach: pathways to representative sampling and appropriate
industry standards. Doctoral Thesis, Esberg, Aalborg University.
Pitard, F. F. 2013. Guidelines for acceptable allotted sampling uncertainty,
Santiago, Gecamin.
Royle, A. G. 1989. Splitting gold assay pulps containing coarse gold particles,
Leeds University Mining Association Journal, 6368.
Royle, A. G. 1991. Safe sampling formulae for gold deposits, Mining
Technology Transactions of the Institutions of Mining and Metallurgy,
100, 8486.
Simon, A. and Gosson, G. 2010. Considerations on QAQC and sampling
security, in Proceedings of Sampling Conference, 135140, Melbourne,
Sketchley, D. A. 1998. Gold deposits: establishing sampling protocols
and monitoring quality control, Exploration and Mining Geology, 7,
129138.
Spangenberg, C. 2011. The status of sampling practice in the gold mining
industry of Africa, in Proceedings of World Conference on Sampling and
Blending, 105112, Santiago, Gecamin.
Valle, M. A. 1998. Sampling quality control, Exploration and Mining
Geology, 7, 107116.
Pitard, F. F. 2015. The advantages and pitfalls of conventional heterogeneity

tests and a suggest alternative, TOS Forum, 5, 1318.
Pitard, F. F. and Franois-Bongaron, D. M. 2011. Demystifying the
fundamental and grouping and segregation error for practitioners, in
Proceedings of World Conference on Sampling and Blending, 3955,
Santiago, Gecamin.
Pitard, F. F. and Lyman, G. 2013. Single and multi-stage Poisson
processes: a case study for gold exploration, in Proceedings of
World Conference on Sampling and Blending, 371385, Santiago,
Gecamin.
Pitard, F. F., Esbensen, K. H. and Paoletti, C. 2015. TOS: progress through
continuity and community, TOS Forum, 4, 2527.
Platten, I. M. and Dominy, S. C. 2003. The occurrence of high-grade gold
pockets in quartz reefs at the Gwynfynydd mine, Wales, United Kingdom:
a geological explanation of the nugget effect, Exploration and Mining
Geology, 10, 249272.
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Date: 20 June 2016, At: 16:52

Importance of good sampling practice

atomic absorption spectroscopy;

HARD half absolute relative difference;

accelerated cyanide extraction;

diamond drill core (diameter of 63.5mm);

blast hole drilling;

incorrect sampling error;

Certified reference material;

diamond drill core (diameter of 48mm);

correct sampling errors;

pulverise and leach;

QA/QC quality assurance/quality control;

gold liberation diameter;

reverse circulation drilling;

screen fire assay;

geological nugget effect;

sampling nugget effect;

gravity recoverable gold;

grouping and segregation error;

Camborne School of Mines, University of Exeter, Penryn, Cornwall,

Dominy Importance of good sampling practice

1998; Spangenberg 2011). The sampling process, inclusive

Nugget effect and TOS

Correct sampling errors

Dominy Importance of good sampling practice

Sampling equipment and materials

Results from grade heterogeneity

Incorrect sampling errors

Defining a representative sample

Results from the incorrect extraction of a sample. Extraction is only

are likely to contribute up to 90%, with DE, extraction error

FSE equation and application to gold ores

Mining Technology 2016VOL. 125NO. 3

Dominy Importance of good sampling practice

Gold mineralisation and sampling

Peculiarities of gold sampling

The following case studies documented between 2001 and

Case study 1: Core quality issues

Dominy Importance of good sampling practice

Case study 2: Incorrect compositing

Case study 3: What coarse gold?

and Platten 2007). These clusters, which may be distributed

Case study 4: Gold segregation in pulps

Mining Technology 2016VOL. 125NO. 3

Dominy Importance of good sampling practice

Case study 5: Grab sampling for grade control

<12cm. Each sample was sent to the laboratory for a 500g

Case study 6: Reverse circulation and blast

Dominy Importance of good sampling practice

During the first few years of operation, all grade control

Case study 7: Uncertainty in heterogeneity

The number of individual fragments should generally be as

Case study 8: Case of QA with no QC

avoiding gold liberation, except during pulverisation