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Sampling for Grinding Pilot Plant

Test – The Effect of Size Distribution
Variability
S Brochot1

ABSTRACT
During the development of a mining project, samples are taken for metallurgical tests. The sample
can be a composite sample made of material coming from a selection of various drilling products
or a sample coming from a mining test. This sample can represent several tonnes of material which
are analysed and split to be used in various tests.
In the current case, a composite sample is dedicated to semi-autogenous grinding (SAG) pilot
plant tests. The property of interest is then the size distribution of the material. The sample is
mixed and a subsample is taken to measure the size distribution which is considered as the feed
size distribution. Then the remaining material of the sample is divided in several subsamples for
batch grinding tests at different operating conditions. The product of each grinding test is then
analysed to measure its size distribution.
The grinding performances are analysed at the light of the measured size distributions for feed
and product. But what is the accuracy of the measurement of these size distributions? What is the
variability of the feed knowing each feed is just a subsample of the initial sample?
The Pierre Gy theory of sampling answers these questions.
The current paper presents, through a real example, the calculation of the measurement error of
the size distributions and the variability of the feed between the different tests. The uncertainties
of the grinding performances are then calculated and their impact on the results interpretation is
then analysed.

INTRODUCTION
During the development of a mining project, samples are
taken for metallurgical tests. The sample can be a composite
sample made of material coming from a selection of various
drilling products or a sample coming from a mining test. This
sample can represent several tonnes of material which are
analysed and split to be used in various tests. In order to take
into account the ore variability in terms of hardness and size
distribution, it is recommended to perform variability studies
(Mosher and Bigg, 2002; Starkey, 2003; Meadows, Scinto and
Starkey, 2011) using samples representing various horizons
or the years of production. But, for a given ore type, it can
be necessary to perform many tests with different operating
conditions. In that case, the variability of the samples is not
due to the heterogeneity of distribution of the deposit, but
only on the heterogeneity of constitution of the primary
sample.
distribution which is considered as the feed size distribution.
Then the remaining material of the sample is divided in
several subsamples which are used as feed of the grinding
tests at different operating conditions. The characterisation
made on the first subsample is used to characterise all the feed
subsamples. That is to say, for example, the same feed size
distribution will be used to calculate the performances of the
different tests even though a variability of the feeds occurs due
to the division stage for obtaining them. The product of each
grinding test is then analysed to measure its size distribution.
As the grinding performances are analysed at the light of
the measured size distributions for feed and product, any
uncertainty in these measurements generates uncertainty in
the performance parameters of the tests and then uncertainty
about the interpretation of results which can be done. Two
questions arise:

In the current case, a metallurgical test campaign is dedicated
to the size reduction stage by semi-autogenous grinding
(SAG). A pilot plant scale SAG mill is used for several batch
tests in various operating conditions. A composite sample
has been taken and constituted on field for this campaign.
The property of interest is then the size distribution of the
material. The sample is mixed and a subsample is taken
for various analyses including the measurement of the size
1. What is the accuracy of the measurement of the size
distributions?
2. What is the variability of the feed knowing each feed is
just a subsample of the initial sample?
The Pierre Gy (1979) theory of sampling answers
these questions. It includes also the question about the
representativeness of the composite sample. Indeed, in the
frame of the development of a mining project, the pertinence

1. Scientific Manager, Caspeo, 3 Avenue Claude Guillemin, BP36009 45060 Orléans CEDEX 2, France. Email: s.brochot@caspeo.net

SAMPLING CONFERENCE / PERTH, WA, 21 - 22 AUGUST 2012 127

S BROCHOT
of the metallurgical tests conducts to the ability of the future
plant to process the ore of the deposit. The composite sample
has to be representative of that deposit, or, at least, of a well
defined part of the deposit or of a specific lithology. The
method to obtain such a representative composite sample
is not the purpose of this paper and is not discussed here.
Consequently, the evaluation of the uncertainty of the
metallurgical tests presented here does not take into account
the uncertainty generated by the constitution of the primary
composite sample. It is why the received primary sample
is considered as the lot (with the meaning of the theory of
sampling) and the point of view is limited to the one of the
metallurgist.
The current paper presents, through a real example, the
calculation of the measurement error of the size distributions
and the feed variability between the different tests. The
first section presents the specificity of the sampling for
particle size distribution analysis. After the definition of
the size distribution, the components of its measurement
error are listed and discussed and a focus is made on the
formulae giving the fundamental sampling error, the main
component in the present case. The formulae giving the
error of the parameters which can be derived from the full
size distribution can then be deduced. The second section
is devoted to the application to the grinding test campaign.
The measurement errors of the characterisation stage are
calculated, as well as the variability of the grinding test
feeds. The uncertainties of the grinding performances are
then calculated and their impact on the results interpretation
is analysed. To conclude, recommendations are proposed
to manage the observed uncertainty and to improve the
metallurgical test representativeness.
SAMPLING FOR PARTICLE SIZE DISTRIBUTION
ANALYSIS
The particle size distribution plays an important role in
the solid material characterisation for many applications in
various industries. It is fundamental in mineral processing
and its measurement is generally the first analysis which
is performed on an ore sample. The performances of many
metallurgical tests will be analysed at the light of the particle
size distribution, not only for the comminution stages for
which the performance parameters are the material fineness
and the reduction ratio, but also for the subsequent processes
such as classification, separation, oxidation, leaching or
smelting.
Focusing on the comminution stage for which the particle
size reduction is observed, it is important to know the accuracy
of the size distribution measurement to be able to judge the
pertinence and discrimination of the various test results.
The particle size distribution can be described with different
parameters such as mean particle size, size of coarsest
particles, size under (or over) which a given percentage
of particles reports, or range of sizes. But, in order to have
a fine description of the behaviour of the ore during the
comminution process, the full particle size distribution is
required. All the cited parameters can be obtained from it.
Mathematically speaking, the size distribution is defined
by a continuous function f (x) where f (x)dx is the weight
proportion of particles having a size between x and x + dx.
The cumulative passing size distribution is the continuous
function F(x) giving the weight proportion of Fi having a size
less or equal to x. It is the primitive of the size distribution
function:
128
x
F (x) = # f (u) du
0
The measurement of the particle size distribution gives only
some points of this cumulative size distribution function. The
size series {xi} of these points depends on the measurement
procedure. If sieving is used to measure the size distribution,
the size series corresponds to the openings of the sieve
series. The particle size is then defined by the ability of the
particle to pass through or to be retained by the sieve mesh.
The definition of the particle size is hardly dependent on the
method of measurement. It is not the aim of this paper to
discuss about this topic and only the sieving method has been
used in the present case. The cumulative size distribution
is then given by the set of weight proportions Fi of particle
having a size less than xi linked to the continuous function by:
x
i
Fi = F (xi) = # f (u) du
0
The particle size classes are defined by the interval between
two successive sieve openings [xi+1; xi [ where the sieves and
the corresponding size classes are numbered from the larger
opening to the smaller one. The first sieve has an opening to
let all the material passing through. If Ns sieves are used for
the size distribution analysis, the size class Ns is the pan and
xNs+1 = 0. The weight proportion of particles in the size class i
is given by: x i
fi = Fi - Fi 1 =
+ # f (u) du
x
i+1
These proportions are measured passing a sample of
material through a sieve stack and then weighing the material
retained in each level. The size class proportion is then the
ratio between the retained mass Mi and the sample mass
Ms. The proportion in the pan is generally calculated as the
remainder. The measurement of the size class proportions
is then a random process generating error at the level of the
sampling stage as well as during analysis.
The sampling error of the size class proportions has
been theoretically treated by Pierre Gy (1979). As the size
distribution is a key factor in the problem of the sampling of
particulate materials, it is generally used to verify the quality
of a sampling plan (Lyman et al, 2010). The consequences
of the overall measurement error of the size distribution on
the calculation of the performances of a process have been
discussed by some authors such as for the hydrocyclone
modelling (Nageswararao, 1999).
Components of the overall measurement error
The absolute measurement error is defined as the difference
between the value of a parameter obtained by a measurement
protocol and the true value which is, by definition, unknown.
The relative measurement error is defined as the ratio between
the absolute measurement error and the true value. In the
following of this paper, the relative error is considered except
when the term ‘absolute error’ is explicitly used.
Due to the natural variability occurring in any measurement
protocol, the measurement error is a random variable
following a probability law which can be obtained using
different approaches. For the statistical approach, the same
measurement is performed a great number of times and
statistics are done on the set of results. The probabilistic
approach is based on theories such as the sampling theory
(Gy, 1979). A combination of these two approaches can be
used to evaluate the overall measurement error.
SAMPLING CONFERENCE / PERTH, WA, 21 - 22 AUGUST 2012
 SAMPLING FOR GRINDING PILOT PLANT TEST – THE EFFECT OF SIZE DISTRIBUTION VARIABILITY
The moments of the probability distribution are used to
characterise the measurement error. The first moment, the
mean, gives an evaluation of the bias, a systematic deviation
between the measurements and the true value. It measures
the accuracy of the measurement. The second moment, the
variance, evaluates the reproducibility (or precision) of the
measurement.
The overall measurement error (OE) includes a lot of
components which can be divided, following the Pierre Gy’s
classification (Gy, 1979), into two main components: the total
sampling error (TE) and the analytical error (AE).
The analytical error is due to the imperfection of the
protocols and devices used for analytical operations. When
concerning size distribution, the analysis is performed on the
primary sample. The evaluation of the analysis error needs
the decomposition of the protocols and procedures to find all
sources of error. Calculation rules and metrological approach
are used to calculate the total analytical error.
The total sampling error has to take into account the
succession of bulk reductions which can occur during the
analysis protocol. It is then the sum of the total sampling
errors at each stage (TEn). The sample preparation operations
generate the preparation error (PE) due to contamination,
loss, chemical or physical alteration, unintentional or
intentional mistakes. The operation of taking a small amount
of material in a lot in order to obtain a sample generates the
sampling error in the proper sense (SE). Its components can
be classified into continuous selection error (CE) resulting
in the immaterial selection of the increments and increment
materialisation error (ME) due to the particulate character
of the material. The components of the continuous selection
error are due to the heterogeneity of the sampled material.
The fundamental sampling error (FE) and the grouping and
segregation error (GE), all together called short-range quality
fluctuation error (QE1), result from the heterogeneity of
constitution, while the long-range (QE2) and periodic (QE3)
quality fluctuation errors, and the weighting error (WE)
comes from the heterogeneity of distribution in the space or
in the time. The increment delimitation error (DE) and the
increment extraction error (EE) constitute the materialisation
error.
Fundamental sampling error of the size class
proportions
The theory of sampling is able to calculate the fundamental
sampling error starting from the description of the
heterogeneity of the material regarding the parameter
to measure: the particle size. The detailed description of
the heterogeneity is deduced from the size and density
distribution analysis. The relative variance of the fundamental
sampling error for the measurement of the content αL of the
critical component in the lot is given by Equation 1:
N and a shape characterised by a shape factor f. The size and
F a -a 2
v 2 (FE) = c 1 - 1 m / miti e i L o (1)
Ms ML aL
i=1
In this formula, Ms is the mass of sample and ML the mass of
the lot. The particles are classified in different heterogeneity
families according to their unit mass, ie the mass of one
particle, and their content of critical component. The NF
families have to be as homogenous as possible, meaning that
all the particles in one family have more or less the same unit
masses, mi, and the same critical component content, αi. ti is
the mass proportion of the family in the lot. This classification
SAMPLING CONFERENCE / PERTH, WA, 21 - 22 AUGUST 2012
in families is called ‘heterogeneity model’. It can be a fancy
of the mind, however based on realistic assumptions. It can
also be obtained from specific experiments characterising
the particles in terms of their heterogeneity. Such a model
of heterogeneity has to be developed for each stage of the
sampling plan. Indeed, the material being classified before
subsampling, the heterogeneity changes in terms of size
distribution.
In the case of the size distribution, the critical component is
one size class of particles and the critical content is that size
class proportion. If the considered size class is entirely and
solely represented by the particles of the family with index c,
Equation 1 becomes:
NF
(FE) = c 1 - 1 mfmc / miti p
1 - 2tc
v2 + (2)
Ms ML tc
i=1
Indeed, the content in the lot αL is the mass proportion of
the considered family tc and the content αi is null for all the
families except for the considered family for which it is one.
The particles of the family c have a size in the range [xc 1; xc [
+
and the particles of the other families have a size outside this
range. Equation 2 gives the relative variance of the fundamental
sampling error for the measurement of the proportion tc of the
size class.
For the same reasons, if the considered size class is entirely
and solely composed of the particles of a set of families with
indexes in the subset Ic⊂{1…NF}, Equation 1 becomes:
NF
v 2 (FE) = c 1 - 1 m f / miti 1 - 2f2 c + / miti p
(3)
Ms ML fc
idI i=1
c
The particles of the families for which iIc have a size in the
range [xc 1; xc [ and the particles of the other families have a
+
size outside this range. Equation 3 gives the relative variance
of the fundamental sampling error for the measurement of
the proportion, fc , of the size class, which is the sum of the
proportions of the families constituting it:
fc = /t i
i d Ic
If the considered size class is too wide in size range, it can
be necessary to cut it into sub size classes with smaller size
ranges assuming a better homogeneity inside each family in
terms of unit mass. Similarly, if the particles in one size class
have various densities or shapes involving a wide range of
unit masses, it can be necessary to use many density or shape
families.
It is common (Gy, 1979) to use size and density classes for
the families used in Equations 1 to 3. Indeed, the size and
density properties of the particles can easily be obtained
experimentally. The shape of the particles can also be taken
into account even though it is more difficult to describe
and estimate it. The particles of one family have then a size
in the range [ya + 1; ya [ , a density in the range [t b; t b+1[
density ranges have to be as thin as possible to minimise the
heterogeneity inside the family. In that case, the particles can
be considered as having a mean size xi and a mean density
t . The unit mass can then be calculated:
i
3
mi = f xi ti
The sieve series {yα} used for the heterogeneity model can
have much more elements than the one {xi} used for analysis,
trying to have {xi}⊂{yα}.
129
S BROCHOT

Analytical error design a sampling plan for size distribution measurement.

If the size distribution analysis is performed many times on Unlike assaying, the sample for size distribution analysis
the same sample, it gives different results demonstrating the cannot be ground. It is why the measurement is directly
random character of the measurement process. Considering performed on the primary sample. For coarse material, the
the sieving method, the variability of the size distribution required primary sample can be so large that it is difficult,
measurement has many sources: even impossible, to analyse the entire sample for all size
classes. Intermediate divisions are then necessary.
• A particle of size x has a probability to pass through
the sieve mesh of aperture α which depends on many
factors. If x > α, this probability is null (by definition of Size distribution parameters
the particle size using sieving method to measure it). But The performances of the metallurgical tests are generally
if x ≤ α the probability is generally less than one. It is small estimated using some parameters calculated from the full size
when the particle size is close to the aperture. The density distribution such as the mean size, the proportion greater or
and the shape of the particles have an influence on this smaller than a given size, the size under or over which reports
probability. The protocol and the operating conditions of a given proportion of material. The first step is to calculate the
the analysis have to be chosen to maximise this probability cumulative size distribution (passing or retained) from the
as close as possible to one. In that case, the variability due individual size distribution. Then, using interpolation on this
to the random behaviour of the particles during sieving is cumulative distribution, other parameters can be calculated
sufficiently reduced. such as the d80, the size under which 80 per cent by weight of
• The protocol and the operating conditions of the analysis the particles report.
have an influence on the results, not only due to their
influence on the probability of classification, but also on Cumulative size distribution
the powder or slurry dispersion, on the recovery of the The fundamental sampling error of the cumulative passing
material in the sieves, on the size fraction drying. size distribution can be derived from the Equation 3:
• The size class proportion being calculated from the Ns NF
1 - 2Fj
mass of the size class fraction relatively to the mass of v 2 (FE) = c 1 - 1 m f / / miti + / miti p (4)
the sample, the variability of the measurement of these Ms ML F j2
c = j i d Ic i=1
masses generates variability in the results.
It is not the purpose of the present paper to obtain the Equation 4 gives the relative variance of the fundamental
analytical error, by calculation or by statistics. Considering sampling error for the measurement of the proportion,
millimetric material, an analytical error of five per cent (two Fj, of the particles smaller than xj, which is the sum of the
sigma) can be used for comparison with fundamental error proportions of the families constituting it:
(Lyman et al, 2010). N N
s s
Fj = / fc = / /ti
Other components c= j c = j i d Ic
As the variance of the grouping and segregation error is safely
taken equal to the one of the fundamental error, the short- Fineness: d80
range quality fluctuation error is twice the fundamental error. The d80 parameter is largely used to characterise the size
The long-range and periodic quality fluctuation errors fineness of material and the performances of comminution and
cannot be accessible through a theoretical approach as the classification processes. It is calculated from the cumulative
degree of mixing of the lot is generally unknown. The simplest passing size distribution by interpolation. As the sieve series
way to calculate these components is to directly observe the follow a geometric progression, a log-linear interpolation is
variability by analysing historical data and, to point out used:
potential issues, by organising a variographic experiment 0.8 - Fi 1
Fi - Fi 1 ^ i + 1)h
(Gy, 1979). It is generally admitted that the weighting error ln (d80) = ln (xi 1) + + ln (x ) - ln (x
+ i
is more or less included in the components of the quality +
fluctuation error when the later is obtained by a variographic
experiment. In the present case, the lot is a primary sample where the index i is chosen to verify Fi + 1 ≤ 0.8 ≤ Fi. The d80 is
for metallurgical tests made of several hundreds of kilograms. then a function of these proportions:
Due to its high value and its relatively small size, it can be d80 = g(Fi; Fi+1)
homogenised and considered as a zero dimension lot for
which the weighting error and the long-range and periodic and the rule of error propagation allows to calculate an
quality fluctuation errors are negligible compared to the approximation of the absolute variance of the measurement
fundamental error. error of the d80:
The delimitation and extraction errors can only be reduced 2g 2 2g 2
v a2 (d80) =
f 2F p va (Fi) + f 2F p va (Fi + 1)
2 2
by using appropriate devices for increment taking, well
designed and well used as it is generally the case in the i i +1
laboratory conditions of a metallurgical test campaign. The relative variance of the d80 is then a function of the
Similarly, the components of the preparation error can only relative variances of the proportions of the cumulative
be reduced by good practice and experimented personnel. passing size distribution:

Sampling plan design ^ ln (xi) - ln (xi+1)h

2 (5)
v 2 (d80) = 6^0.8 - Fi + 1h Fi v (Fi) +
2 2 2
If the fundamental error is the main component of the overall (Fi - Fi + 1) 4
measurement error of the size distribution, as it is frequently
^ Fi - 0.8h Fi + 1v (Fi + 1) @
the case for coarse material, its calculation can be used to 2 2 2

130 SAMPLING CONFERENCE / PERTH, WA, 21 - 22 AUGUST 2012

 SAMPLING FOR GRINDING PILOT PLANT TEST – THE EFFECT OF SIZE DISTRIBUTION VARIABILITY

PILOT PLANT CAMPAIGN OF GRINDING TESTS
The metallurgical tests have been performed on a lateritic
ore which is a blend of limonite, earthy saprolite and rocky
saprolite facies. Limonite and earthy saprolite are characterised
by a large proportion of -100 μm, earthy saprolite having a
larger proportion of millimetric particles. Rocky saprolite is
characterised by a large proportion of +10 mm.
The metallurgical test campaign is focused on the size
reduction stage by semi-autogenous grinding (SAG). A
pilot plant scale SAG mill is used for several batch tests in
various operating conditions. A primary sample of 5615 kg
(wet mass) coming from the deposit is used to perform these
tests. The representativeness of this sample relatively to the
deposit is not discussed in this paper. The primary sample
is then considered as the lot and only the subsampling for
characterisation and the feed variability between the tests are
studied here.
The primary sample is prepared following the procedure:
1. unloading and homogenisation with a front-end loader
2. division by coning and quartering to obtain a subsample
of 352 kg (wet mass)
3. drying of the subsample in oven for moisture content
measurement: 279 kg (dry mass) – 20.7 per cent moisture
4. division of the dried subsample to obtain 137 kg for
sample characterisation
5. crushing down to -1 mm of the remaining part of the step 4
and division by a sample splitter to obtain three samples
for head assay
6. division by coning and quartering of the remaining part
of the step 2 to obtain a set of subsamples for the grinding
tests.
The products of the grinding tests are characterised in order
to calculate the grinding performances.
Feed characterisation
The primary sample is characterised through a subsample
issued from the step 4 of the preparation procedure of the
primary sample. The results of this analysis are used as feed
characterisation for all the grinding tests performed with the
primary sample material. The analyses performed on the
subsample of 137 kg are:
• Size distribution analysis by sieving with screen opening
100 mm, 50 mm, 11.2 mm, 5 mm, 2.8 mm, 1.4 mm and
0.1 mm. The larger particles are less than 200 mm. A
sample of the -0.1 mm fraction is taken and analysed by
laser diffraction for the fine size distribution.
• Each size fraction is crushed down to -1 mm if necessary
and divided using a sample splitter. Subsamples of the
size fractions are assayed by XRF.
• The three subsamples obtained from the step 5 of the
preparation procedure of the primary sample are assayed
by XRF.
The equivalent dry mass of the lot is then ML = 4453 kg.
The mass of sample for particle size analysis is MS = 137 kg.
The masses of material recovered in each size fraction are
given in the Table 1 as well as the size class proportions and
their associated relative fundamental sampling error (RFSE)
calculated as two times the standard deviation (with 95 per
cent confidence) obtained from Equation 2.
The large fundamental sampling error for the measurement
of the 100 - 200 mm size proportion is due to the small number
of particles in the sample size fraction, three or four, in this
class. In that case, the approximation done to obtain the
Equation 2 is not valid. It is necessary to return to the primary
formulae based on Poisson distribution of particle numbers
(Gy, 1979; Lyman et al, 2010). It can be the case also for the two
following size classes for which the number of particles in the
sample size fractions is <1000. The large error, 16.2 per cent,
for the smallest size classes is a consequence of the influence
of the coarsest size classes in their representativeness.
The two last columns of the Table 1 give the proportions of
the cumulative passing size distribution and their associated
relative fundamental sampling error. The d80 calculated by
log-linear interpolation is 90 mm. The associated relative
fundamental sampling error calculated with Equation 5 is
15 per cent or 14 mm as absolute error.
Variability of test feeds
The material used for each grinding test is a subsample of the
primary sample obtained from the step 6 of the preparation
procedure of the primary sample. As any sampling process,
it is subjected to variability. Once again, the fundamental
sampling error gives the amplitude of this variability. The
mean size distribution of the test feeds is supposed to be
the one measured from the characterisation subsample as
described above.
The masses of material fed in the SAG mill vary from 58 kg
to 146 kg. The Table 2 gives the size class proportions and
their associated relative fundamental sampling error (with
95 per cent confidence) for these two extremes.

TABLE 1
Sample size distribution.

Size class ranges Weights (g) Proportions (%) Relative fundamental Cumulative passing Relative fundamental
(mm) sampling error of proportions (%) sampling error of
proportions (%) cumulative passing
proportions (%)
100 - 200 17 650 12.87 90.9 100.00 0.0
50 - 100 63 340 46.18 17.0 87.13 13.5
11.2 - 50 15 760 11.49 18.4 40.95 16.2
5 - 11.2 1399 1.02 16.8 29.46 16.2
2.8 - 5 798 0.58 16.3 28.44 16.2
1.4 - 2.8 676 0.49 16.2 27.86 16.2
0.1 - 1.4 3632 2.65 16.2 27.36 16.2
-0.1 33 900 24.72 16.2 24.72 16.2
Total 137 155 100.00

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S BROCHOT

TABLE 2
Test feed size distribution variability.

Size class ranges (mm) Proportions (%) Relative fundamental sampling Relative fundamental sampling
error of proportions (%) 58 kg of error of proportions (%) 146 kg
feed of feed
100 - 200 12.87 141.0 88.0
50 - 100 46.18 26.4 16.5
11.2 - 50 11.49 28.5 17.8
5 - 11.2 1.02 26.0 16.3
2.8 - 5 0.58 25.2 15.8
1.4 - 2.8 0.49 25.1 15.7
0.1 - 1.4 2.65 25.0 15.6
-0.1 24.72 25.0 15.6

Here also, the large fundamental sampling error for the
100 - 200 mm size proportion is due to the small number of
particles in this feed size fraction, one or two for 58 kg and
three or four for 146 kg. The large error, 25.0 per cent for 58 kg
and 15.6 per cent for 146 kg, for the smallest size classes is also
a consequence of the influence of the coarsest size classes in
their variability.
The uncertainty of the size distribution of the test feed due to
its overall measurement error adds to the intrinsic variability
of the feed as it is itself a sample. The sampling process for
the characterisation and the sampling process for the test feed
are not really independent as they are taken in the same lot
without replacement. Nevertheless, the variance of the global
uncertainty of the feed size distribution can be approached
by the sum of the variance of the overall measurement error
of the size distribution and the variance of the fundamental
sampling error for test sampling.
The Table 3 gives the proportions of the cumulative passing
size distribution and their associated uncertainty for the
extremes of feed mass. The variance of the uncertainty is
the sum of the variance of the fundamental sampling error
for characterisation and of the variance of the fundamental
sampling error for test sampling. The analytical error has
not been taken into account. The uncertainty of the feed d80
calculated with the Equation 5 is 27.6 per cent for 58 kg and
20.8 per cent for 146 kg (respectively 25 mm and 19 mm as
absolute error).
Product characterisation
Once the grinding test performed, the mill product is entirely
analysed for size distribution. Consequently, there is no
sampling error. The overall measurement error is limited
to the analytical error. The d80 of the grinding test products
varies from 24 mm to 77 mm and one test gives a product d80
of 92 mm. This apparently abnormal result giving a product
coarser than the feed (d80 of 90 mm) can be explained by the
large uncertainty of the feed d80. Indeed, the concerned test
was performed with only 71 kg which give an uncertainty
of 25.8 per cent that is to say a feed d80 which can vary from
66 mm to 114 mm. Considering a five per cent analytical error
for the measurement of the product size distribution, there is
a seven per cent error for the product d80 which can vary from
85 mm to 99 mm.
Consequence regarding interpretation of
results
The test giving the coarsest product with a d80 of 77 mm
has been performed with a sample of 72 kg. The calculated
uncertainty on the feed d80 is then 25.6 per cent. The reduction
ratio is 1.17. Taking into account the feed uncertainty and the
analytical error of the product size distribution, the error of
the reduction ratio is 26.5 per cent.
The test giving the finer product with a d80 of 24 mm has been
performed with a sample of 79 kg. The calculated uncertainty
on the feed d80 is then 24.9 per cent. The reduction ratio is 3.74
with an error of 25.8 per cent.
Another way to measure the grinding performances is to
calculate the operating work index:
W
Wi =
10 - 10
dP80 dF80

TABLE 3
Test feed cumulative passing size distribution uncertainty.

Size class ranges (mm) Cumulative passing proportions Uncertainty of cumulative passing Uncertainty of cumulative passing
(%) proportions (%) 58 kg of feed proportions (%) 146 kg of feed
100 - 200 100.00 0.0 0.0
50 - 100 87.13 24.8 18.7
11.2 - 50 40.95 29.9 22.5
5 - 11.2 29.46 29.8 22.5
2.8 - 5 28.44 29.8 22.5
1.4 - 2.8 27.86 29.8 22.5
0.1 - 1.4 27.36 29.8 22.5
-0.1 24.72 29.8 22.5

132 SAMPLING CONFERENCE / PERTH, WA, 21 - 22 AUGUST 2012


where W is the specific energy consumed during the test, dF80
and dP80 are respectively the feed and product d80. Considering
the specific energy as perfectly known (which is far from the
reality but the objective here is to know the influence of the
size distribution uncertainty on the operating work index
estimate), the uncertainty relative variance on the operation
work index, calculated using the rule of error propagation (for
the large errors used here, this rule start to be inapplicable),
is given by:
d v 2 (dP80) + dP80 v 2^dF 80h
v 2 (wi) = F 80
4 ` dF 80 - dP80 j
2
For the test giving the coarsest product, the calculated error
on the operating work index is 166 per cent while it is 15.2 per
cent for the test giving the finest product.
Four tests have been conducted with different per cent-
solids, 25 per cent, 30 per cent, 40 per cent and 50 per cent,
the other operating conditions being constant. Table 4 gives,
for each of these four tests, the mass of sample used, the d80
of the product, the reduction ratio and its associated error,
and the operating work index and its associated error. The
Figure 1 displays the variation of the reduction ratio and of
the operating work index with the per cent-solids. The error
bars correspond to one standard deviation (half error).
40
Operating work index
Reduction ratio
30
Operating work index (kWh/t)
20
10
0 1
20 30 40
%-solids
FIG 1 - Variation of reduction ratio and operating work index with
per cent-solids.
It clearly shows the difficulty to conclude about the influence
of the per cent solids on these performance parameters.
If one can say the operating work index and the reduction
ratio are respectively increasing and decreasing with the per
cent-solids, it is not possible to conclude about an apparent
extreme around 30 per cent solids.
The ore mentioned here presents a chemical and mineral-
ogical composition which depends on the particle size. The
uncertainty observed for the size distribution reports to
the composition uncertainty. Consequently, the separation
Solid content (%) Sample mass (kg)
25 58
30 74
40 97
50 126
SAMPLING CONFERENCE / PERTH, WA, 21 - 22 AUGUST 2012
SAMPLING FOR GRINDING PILOT PLANT TEST – THE EFFECT OF SIZE DISTRIBUTION VARIABILITY
and enrichment processes following the grinding stage are
impacted.
CONCLUSIONS
The main result of this sampling approach to estimate the
validity of metallurgical test works is the large uncertainty
at the level of the primary sample characterisation as well
as the variability of the feed of the different tests. And this
uncertainty does not account the uncertainty in the primary
sample representativeness. Even though this observation
seems pessimistic it has not to question the results of the
conducted metallurgical tests. Indeed, the specificity of
the ore has well been taken into account. The results of this
first campaign have been confirmed by another one, at least
concerning the behaviour of the ore during grinding. But
all the results have to be read at the light of the mentioned
uncertainty. That is to say, if some relationships are observed
between performance parameters and operating conditions,
they have to be compared to the expected ones. If the
differences are compatible with the level of uncertainty, the
simplest relationships have to be chosen. Conversely, if the
observed behaviour is far from the expected one or if the
relationships do not appear clearly, the uncertainty analysis
has to discriminate between a bad test (issue during operation
or analysis), a specific behaviour of the ore, or a result due to
1.8
variability.
Nevertheless, concerning the pilot plant test campaign
described here, the following improvements can be mentioned
1.6 for recommendations:
• Perform the size distribution analysis on a larger sample.
If the 279 kg of sample obtained in the step 3 of the
Reduction ratio
1.4 sample preparation procedure are analysed, the relative
fundamental sampling error of the coarsest class decreases
to 63 per cent (with a too small number of particles) and
1.2 of the finest to 11.2 per cent. Unfortunately, this has only
a small impact on the d80 error which decreases from
27.6 per cent to 25.4 per cent for 58 kg and from 20.8 per
cent to 17.8 per cent for 146 kg.
50 • As the main component of the uncertainty is coming from
the variability of the test feeds, each feed can be analysed
for the size distribution before performing the test and
then homogenised after the blending of the size fractions.
This has the advantage of avoiding the sampling error of
the characterisation stage and of using the ‘true’ feed size
distribution to calculate the grinding test performances.
The main disadvantage is the increase in material handling
and then in time and cost.
• As head assays and size by size assays have been done for
the feed and the products, data reconciliation by material
balance can be conducted to improve the accuracy of the
determination of the size distribution thanks to the better
accuracy of assaying. Combined with some assumptions
concerning the breakage matrix, some uncertainties can be
reduced.
TABLE 4
Comparison of test results for various per cent-solids.
Product d80 (mm) Reduction ratio Reduction ratio Operating work Operating work
error (%) index (kWh/t) index error (%)
63 1.43 28.5 21.8 74.2
61 1.47 26.3 15.2 62.5
70 1.28 24.3 19.5 92.5
81 1.11 22.7 35.9 214.4
133
S BROCHOT
The approach presented here for the grinding tests can be
applied for any kind of metallurgical test. The same question
of representativeness can be done for laboratory test such as
the determination of the Bond work index or of the breakage
matrix.
The results of such metallurgical test works are used
to design and scale up the future processing plant. The
uncertainty at the pilot plant scale has to be propagated to
the full-scale calculation and introduced in the financial risk.
Such an uncertainty analysis, conducted during prefeasibility
or feasibility study, also helps in the definition of the future
metallurgical tests to reduce the uncertainty and to answer
some questioning. This approach can also be done before the
first metallurgical tests. It is a way to have a better choice in
the operating conditions to test and to select the more relevant
ones. Indeed, it is always preferable to conduct less tests but
with a better accuracy.
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SAMPLING CONFERENCE / PERTH, WA, 21 - 22 AUGUST 2012