CHAPTE R 1

Mineral Sampling
1.1 Introduction
A processing plant costs many millions of dollars to build and operate. The success of this
expenditure relies on the assays of a few small samples. Decisions affecting millions of
dollars are made on the basis of a small fraction of the bulk of the ore body. It is therefore
very important that this small fraction is as representative as possible of the bulk material.
Special care needs to be taken in any sampling regime, and a considerable effort in statis-
tical analysis and sampling theory has gone into quantifying the procedures and precau-
tions to be taken.
The final sampling regime adopted is, however, a compromise between what theory tells us
should be done and the cost and difficulty in achieving this in practice.

1.2  Statistical Terminology

A measurement is considered to be accurate if the difference between the measured value and
the true value falls within an acceptable margin. In most cases, however, the true value of the
assay is unknown, so the confidence we have in the accuracy of the measured value is also
unknown. We have to rely on statistical theory to minimise the systematic errors to increase
our confidence in the measured value.
Checks can be put in place to differentiate between random variations and systematic errors
as the cause of potential differences. A random error (or variation) on average, over a period
of time, tends to zero, whereas integrated systematic errors result in a net positive or negative
value (see Figure 1.1).
The bias is the difference between the true value and the average of a number of experimental
values and hence is the same as the systematic error. The variance between repeated samples
is a measure of precision or reproducibility. The difference between the mean of a series of
repeated samples and the true value is a measure of accuracy (Figure 1.2).
A series of measurements can be precise but may not adequately represent the true value.
Calibration procedures and check programs determine accuracy and repeat or replicate/
duplicate measurements determine precision. If there is no bias in the sampling regime, the
precision will be the same as the accuracy. Normal test results show that assays differ from
sample to sample. For unbiased sampling procedures, these assay differences are not due to
Mineral Processing Design and Operations
http://dx.doi.org/10.1016/B978-0-444-63589-1.00001-0 1 Copyright © 2016 Elsevier B.V. All rights reserved.
2  Chapter 1

Figure 1.1: Representation of a Random and Systematic Error.

any procedural errors. Rather, the term ‘random variations’ more suitably describes the vari-
ability between primary sample increments within each sampling campaign.
Random variations are an intrinsic characteristic of a random process, whereas a systematic
error or bias is a statistically significant difference between a measurement, or the mean of a
series of measurements, and the unknown true value (Figure 1.1). Applied statistics plays an
important role in defining the difference between random variations and systematic errors and
in quantifying both.

1.2.1 Mean

The most important parameter for a population is its average value. In sampling and weigh-
ing the arithmetic mean and the weighted mean are most often used. Other measures for the

Figure 1.2: Difference Between Precision and Accuracy.

 Mineral Sampling  3

Figure 1.3: Normal Distribution.

average value of a series of measurements are the harmonic mean, and the geometric mean.
Mode and median are measures of the central value of a distribution. The mode forms the
peak of the frequency distribution, while the median divides the total number of measure-
ments into two equal sets of data. If the frequency distribution is symmetrical, then its mean,
mode and median coincide as shown in Figures 1.3 and 1.4.
For a binomial sampling unit of mixed particles, the average percentage of mineral A is cal-
culated by adding up all measurements and by dividing their sum by the number of measure-
ments in each series.

x=
∑x i
(1.1)
n

Figure 1.4: Asymmetric Distribution.

4  Chapter 1

where
x  = sample mean (arithmetic)
xi = ith measurement
n = number of increments
The weighted percentage is calculated, either from the total number of particles in each
series, or by multiplying each incremental percentage with the mass in each corresponding
increment, and by dividing the sum of all products by the total mass for each series. However,
the small error that is introduced by calculating the arithmetic mean rather than the weighted
average is well within the precision of this sampling regime. The following formula is used to
calculate the weighted average for a sample that consists of n primary increments:

x=
∑ ( ∆M ⋅ x )
i i
(1.2)
M
where
∆Mi = mass of ith increment
M = mass of gross sample
Due to random variations in the mass of each primary increment the weighted average is a
better estimate of v, the unknown true value, than the arithmetic mean.

1.2.2 Variance

The variance, and its derived parameters such as the standard deviation and the coefficient of
variation, are the most important measures for variability between test results.
The term range may be used as a measure of variability.

Example 1.1
Consider a binary mixture of quartz and hematite particles with approximately 10% hematite.
Samples are taken and the number of hematite particles is counted to obtain the percentage of
hematite in the sample. Table 1.1 gives the result of 10 samples. For a binomial sampling unit
the range is (maximum value – minimum value) = 12.6 − 5.7 = 6.9%.
If each series of measurements is placed in ascending order, then the range is numerically
equal to xn − x1 so that the range does not include information in increments x2, x3, …, xn−l.
For a series of three or more measurements the range becomes progressively less efficient as a
measure for variability as indicated in Figure 1.5.
For two samples, the range is the only measure for precision but this is not sufficient to estimate
the precision of a measurement process. The precision of a measurement process requires the
mean of absolute values of a set of ranges calculated from a series of four or more simultaneous
duplicates. This is the variance.
 Mineral Sampling  5

Table 1.1: Sampling of a binary mixture with a binomial population (quartz and hematite).
Sample
Number Quartz Hematite Total % Hematite

1 105 11 116 9.5

2 132 19 151 12.6
3 99 10 109 9.2
4 98 7 105 6.7
5 83 5 88 5.7
6 87 11 98 11.2
7 91 12 103 11.7
8 86 8 94 8.5
9 98 12 110 10.9
10 113 14 127 11.0

Figure 1.5: Range of Experimental Values.

The classical formula for the calculation of the variance is

(∑ x )
2

∑x
i
2
−
var( x ) =
∑(x − x ) i
2

≈
i
n (1.3)
n −1 n −1
where
n = number of measurements
n − 1 = degrees of freedom
The standard deviation, σ, is the square root of the variance. The coefficient of variation (CV)
is a measure of precision and is numerically equal to

100 σ
CV(%) = (1.4)
x
6  Chapter 1

Table 1.2: Variance values from sampling a binary mixture of quartz and hematite.
Small Increment Large Increment
Number Quartz Hematite Total % Hematite Quartz Hematite Total % Hematite

1 105 11 116 9.48 504 53 557 9.52

2 132 19 151 12.58 350 45 395 11.39
3 99 10 109 9.17 597 56 653 8.58
4 98 7 105 6.67 394 52 446 11.66
5 83 5 88 5.68 428 43 471 9.13
6 87 11 98 11.22 438 52 490 10.61
7 91 12 103 11.65 508 55 563 9.77
8 86 8 94 8.51 533 56 589 9.51
9 98 12 110 10.91 438 50 488 10.25
10 113 14 127 11.02 490 49 539 9.09
SUM 96.89 SUM 99.51
Arithmetic mean 9.69 Arithmetic mean 9.95
Variance 5.0141 Variance 1.1264
Standard deviation 2.2392 Standard deviation 1.0613
Coeff. of variation 23.1 Coeff. of variation 10.7

Example 1.2
Variance values from a sampling procedure with a binary mixture of mineral particles are given
in Table 1.2.

The physical appearance of a sample that consists of 50 primary increments of 5 kg each is
similar to that of a sample containing five increments of 50 kg, or to that of 250 kg of a bulk
solid. However, the difference in intrinsic precision (as indicated by the variance) may be
dramatic, particularly if the variability within the sampling unit is high.
In practical applications of sampling bulk solids we compromise by collecting and measuring
unknown parameters on gross samples, and by reporting x , the sample mean as the best esti-
mate for v, the unknown true value. If all increments are contained in a single gross sample,
we have no information to estimate the precision of this sampling regime. If we want to know
more about the precision of samples, systems and procedures, it is essential that duplicate or
replicate measurements be made, from time to time, to determine the coefficient of variation
for each step in the chain of measurement procedures.

1.2.3  Confidence Intervals

Other convenient measures for precision are confidence intervals (CI) and confidence ranges
(CR). 95% confidence intervals and 95% confidence ranges may be used, although if concern
over sampling precision is high, then 99% or 99.9% confidence limits must be considered.
 Mineral Sampling  7

That is, if we repeat a particular experiment 100 times, then 95 times out of 100 the
results would fall within a certain bound about the mean and this bound is the 95%
confidence interval. Similarly, confidence limits of 99% and 99.9% mean that 99 times
out of 100, or 999 times out of 1000 measurements, would fall within a specified or
known range.
In the draft Australian Standard, DR00223, for estimating the sampling precision in sampling
of particulate materials, a confidence interval of 68% is chosen [1].
Fortunately, we do not need to repeat a measurement 100 times if we want to determine its
95% confidence interval, either for individual measurements or for their mean. Applied sta-
tistics provides techniques for the calculation of confidence intervals from a limited number
of experiments. The variance between increments, or between measurements, is the essential
parameter.
The most reliable estimate of σ2 is var(x), the variance of the sample. The reliability of this
estimate for σ2 can be improved by collecting, preparing and measuring more primary incre-
ments, or by repeating a series of limited experiments on the same sampling unit.
The 95% confidence interval for a normal distribution is equal to ±1.96σ from the distribu-
tion mean. In practice, we often use the factor 2 instead of 1.96 to simplify calculations and
precision statements. The 68% confidence interval is equal to ±0.99σ, for infinite degrees of
freedom and if the number of replicate results exceeds 8 then a factor of 1.0 is an acceptable
approximation.

1.3  Mineral Particles Differing in Size – Gy’s Method

Representing large bodies of minerals truly and accurately by a small sample that can be
handled in a laboratory is a difficult task. The difficulties arise chiefly in ascertaining a proper
sample size and in determining the degree of accuracy with which the sample represents the
bulk sample.
In each case, the accuracy of the final sample would depend on the mathematical probability
with which the sample represents the bulk material. The probability of true representation
increases when incremental samples are taken while collecting from a stream, like a conveyor
belt for solids and off pipes for liquids or slurries.
Several methods have been put forward to increase the probability of adequately representing
the bulk minerals [2–5]. One such method involving both the size and accuracy of a sample
taken for assay was developed by Gy and is widely used [6,7]. Gy introduced a model based
on equiprobable sample spaces and proposed that if
dMAX = dimension of the largest particle
MMIN = minimum mass of sample required
8  Chapter 1

σ2 = variance of allowable sampling error in an assay (in the case of a normal distribution
this equals the standard deviation)
then
3
Kd MAX
M MIN = (1.5)
σ2

where K is usually referred to as the sampling constant (kg/m3).

In mineralogical sampling the dimension of the largest piece (dMAX) can be taken as the screen
aperture through which 90–95% of the material passes. As ±2σ represent the probability of
events when 95 out of 100 assays would be within the true assay value, 2σ is the acceptable
probability value of the sample. The sampling constant K is considered to be a function of the
material characteristics and is expressed by

K = PS PD PL ⋅ m (1.6)

where
PS = particle shape factor (usually taken as 0.5 for spherical particles, 0.2 for gold ores)
PD = particle distribution factor (usually in the range 0.20–0.75 with higher values for nar-
rower size distributions, usually taken as 0.25 and 0.50 when the material is closely sized)
PL = liberation factor (0 for homogeneous (unliberated) materials, 1 for heterogeneous
(liberated) and see Table 1.3 for intermediate material)
m = mineralogical factor
The mineralogical factor, m, has been defined as

(1 − α ) 
m =  [(1 − α ) ρM + αρG ] (1.7)
 α 

where
a = the fractional average mineral content and
ρM and ρG = the specific gravity of the mineral and the gangue, respectively
The liberation factor, PL, is related to the top size dMAX and to the liberation size dL of the min-
eral in the sample space. It can be determined using Table 1.3. In practice, PL is seldom less
than 0.1 and if the liberation size is unknown then it is safe to take PL as 1.0.

Table 1.3: Liberation factors as a function of liberation size [8].

Top Size/Liberation
Size, (dMAX/dL) <1 1–4 4–10 10–40 40–100 100–400 >400

Lib. Factor (PL)) 1.0 0.8 0.4 0.2 0.1 0.05 0.02
 Mineral Sampling  9

When a large amount of sample has been collected, it has to be split by a suitable method
such as riffling. At each stage of subdivision, samples have to be collected, assayed and
statistical errors determined. In such cases, the statistical error for the total sample will be the
sum of the statistical errors during sampling (σS) and the statistical error in assay (σA), so that
the total variance ( σ T2 ) will be

σ T2 = σ S2 + σ A2 (1.8)

When the sample is almost an infinite lot and where the proportion of mineral particles has
been mixed with gangue and the particles are large enough to be counted, it may be easier to
adopt the following procedure for determining σP.
Let
PM = proportion of mineral particles
PG = proportion of gangue particles
N = number of particles
Then, the standard deviation of the proportion of mineral particles in the sample, σP, will be

PM PG
σP = (1.9)
N

The standard deviation on a mass basis (σM) can be written in terms of the percent mineral in
the whole sample, provided the densities (ρ) are known. Thus if ρM and ρG are the densities
of the mineral and gangue, then the mass percent of mineral in the entire sample, consist-
ing of mineral and gangue (the assay), will be
100 PM ρ M
AM = (1.10)
PM ρ M + PG ρG

assuming that the particles of mineral and gangue have the same shape and size.
dAM
The standard deviation of the entire sample is given by σ T = ⋅ σ P or
dP

 (100 − AM ) ρ M + AM ρG  AM (100 − AM )
σT =  ⋅ (1.11)
 100 ρ M ρG  N

Example 1.3
Regular samples of the feed were required at a copper-processing plant, having a copper
content of about 9%. The confidence level of estimation was required to be 0.1% Cu at 2σ
10  Chapter 1

standard deviation. The liberation size of the Cu mineral (chalcocite) in the ore was determined
to be 75 mm. The top size of the ore from the sampler was 2.5 cm. Determine the minimum
mass of sample required to represent the ore, given that the density of chalcocite is 5600 kg/m3
and the density of the gangue is 2500 kg/m3.

Solution
From the data, dMAX = 2.5 cm.
Since the confidence interval required is equal to ±0.1% of a 9% assay,

2σ = 0.1/ 9 or σ = 0.011/ 2 = 0.00555

Again from the data dMAX/dL = 25/0.075 = 333.33; hence from Table 1.3, PL = 0.05.

As the ore contains chalcocite (Cu2S) assaying about 9% Cu, it can be considered to contain
[159.2/(63.56 × 2)] × 9 = 11.3% of Cu2S. Thus a = 0.113.
That is, the copper content of Cu2S is given by the ratio of atomic masses

(63.56 × 2) × 100 127.1× 100

= = 79.8% Cu (atomic mass, Cu = 63.56, S = 32.1)
(63.56 × 2) + 32.1 159.2

The chalcocite content of the ore is then given by

9 × 100
= 11.3%
79.8

The mineralogical composition factor, m, can now be calculated from Equation (1.7),

 (1− α ) 
m= (1− α ) ρM + αρG 
 α 

 (1− 0.113) 
m= [(1− 0.113) 5600 + (0.113 × 2500)] = 41,207.8kg/m3
 0.113 

then from Equation (1.6)

K = 0.5 × 0.25 × 0.05 × 41,207.8 = 257.5kg/m3 and

MMIN = [257.5 × (0.025)3 ] / (0.00555)2 = 130.6kg

Thus, the minimum sample size should be 131 kg.

Note the importance of not rounding off the numbers until the final result. If σ is rounded to
0.0055, then MMIN = 133 kg and if σ is rounded to 0.0056 then MMIN = 128 kg.
 Mineral Sampling  11

Example 1.4
A composite sample of galena and quartz was to be sampled such that the assay would
be within 0.20% of the true assay, of say 5.5%, with a probability of 0.99, i.e. the sample
assay would be 5.5% ± 0.20%, 99 times out of 100. Given that the densities of galena and
quartz were 7400 kg/m3 and 2600 kg/m3, respectively, and the average particle size was
12.5 mm with a mass of 3.07 g, determine the size of the sample that would represent the
composite.

Solution
Step 1
Determine σT in terms of N from Equation (1.11).

 (100 − 5.5) 7400 + 5.5 × 2600  5.5 (100 − 5.5)

σT =  
 100 7400 × 2600 N
(1.12)
37.089
=
N

To determine N it is necessary to find σT

Step 2
To determine the value of σT to satisfy the deviation limits so that the area under the curve
between the limits will be 99% of the total area, use Table 1.4.
From the table, corresponding to a probability of 0.99, the value of the deviation from the
standard unit is 2.576.
i.e.

x x 0.20
X= or σ T = = = 0.07764
σT X 2.576

Table 1.4: Probability P vs. deviation X, relative to unit standard deviation [9].
Deviation from Standard Deviation from Standard
Unit, X Unit, X
Probability p X = x/σT Probability p X = x/σT

0.90 1.645 0.97 2.170

0.91 1.705 0.98 2.326
0.92 1.750 0.99 2.576
0.93 1.812 0.999 3.291
0.94 1.881 0.9999 3.890
0.95 1.960 0.99999 4.417
0.96 2.054 0.999999 4.892
12  Chapter 1

Substituting into Equation (1.12), N = (37.089/0.07764)2 = 228,201.9.

Hence, the mass of sample necessary to give an assay within the range 5.5 ± 0.20%, 99 times
out of 100 would be = 228,201.9 × 3.07 = 700,579 g ≈ 701 kg.

1.4  Mineral Particles of Different Density

Where variations in density of individual particles and their composition occur, the following
considerations may be adopted to provide the sample size [9]:
1. Divide the material into n density fractions, ρ1, ρ2, ρ3, …, ρn varying from purely one
mineral to the other, e.g. copper and quartz in a copper ore, and consider n size fractions,
d1, d2, d3, …, dn.
2. Consider the mass percent of the ith size fraction and jth density fraction as Mij.
3. Consider Aij and Pij as the assay and the proportion of particles in the ith size and jth den-
sity fractions.
For sampling a mixture of two components (mineral and gangue) the proportion of particles
in the ij fraction would be
Mij / di3 ρ j
Pij = (1.13)
∑(M ij / di3 ρ j )
And the assay of the mixture, Aij, will be approximately equal to

 ρ M ( ρij − ρG )100 
Aij =  (1.14)
ρij ( ρ M − ρG )

where
ρM = density of the mineral and
ρG = the density of the gangue
and the standard deviation of the ijth fraction will be
Pij (1 − Pij )
σ2 = (1.15)
N

For a multi-component system the principles developed in Equations (1.13)–(1.15) may be

extended. Their solution can be achieved easily by a computer. The general equation for
overall sample assay is

∑d P ρ A 3
i ij j ij
ij
Aij = (1.16)
∑d P ρ 3
i ij j
ij
 Mineral Sampling  13

Example 1.5
A nickel sulphide ore mineral (pentlandite) has an average particle size of 1 mm. It is separated
into three fractions and the properties of each fraction are as follows:

Fraction Mass (%) Assay (% pentlandite) Density

1 (Concentrate) 2.4 100.0 4.8
2 (Middlings) 81.0 58.9 3.6
3 (Tail) 16.6 0.0 2.65

The lot has to be sampled so that it would assay ±0.15% of the true assay having 5% with a
probability of 99%.
Solution
Step 1.
As the stipulated probability is 0.99, Table 1.4 may be used.
Here

0.15
X= = 2.576 or σ = 0.058
σ
Step 2.
Estimate Pij from Equation (1.13) in the following manner (Table 1.5).
Step 3.
Pi (1− Pi )
With known P and σ, N can be estimated using the equation σ 2 =
N
Now follow Example 1.4 to determine the sample size.

Table 1.5: Calculation of proportion of particles in the ijth fraction.

Mass % Proportion
Fraction Mass Assay SG Av. Dia di3 di3 × ρ di3 · ρ by No.
I j % di (7) × (5) (3)/(8) (9)/9
(1) (2) (3) (4) (5) (6) (7) (8) (9) (10)
1 1 2.4 100.0 4.8 1 1 4.8 0.5 0.017
1 2 81.0 58.9 3.6 1 1 3.6 22.7 0.776
1 3 16.6 0.0 2.65 1 1 2.65 6.03 0.207
 100.0 29.23 1.0
14  Chapter 1

1.5  Incremental Sampling

Theoretically, unbiased gross samples can be obtained by collecting a sufficiently large
number of single particles from a sampling unit. If each particle has a finite chance of being
selected for a gross sample, and if this probability is only a function of its size, then this col-
lection of particles will constitute an unbiased probability sample.
In the practice of sampling bulk solids, such a sample collection scheme is highly impractical.
Therefore, we collect groups of particles for primary increments.
Sampling experiments that are based on the collection of a series of small and large incre-
ments from a large set of particles demonstrates that the precision of a single-increment
sampling regime is a function of the number of particles in a primary increment. As a mat-
ter of fact, the formula for the variance of a binomial sampling unit, var(x) = N·p·q, shows
the fundamental relationship between probabilities (p, q), the total number of particles in an
increment (N), and thus its mass, and the precision for the parameter of interest. Hence, the
precision of a single increment is essentially determined by its mass.
The binomial sampling experiment in which p = 0.095 and q = 0.905 (q = alternate binomial
probability = 1 − p) can be used to set up a table in which the precision of a primary incre-
ment is given as a function of the average number of particles in an increment. In Table 1.6,
the 95% confidence ranges (CR) that are calculated from corresponding 95% confidence in-
tervals (CI) for the expected number of value particles in each increment, together with their
coefficients of variation, are listed.
Since these ranges are based on properties of the binomial distribution, their values are obvi-
ously independent of particle size. For a bulk solid with a certain density, its top size deter-
mines the mass of a primary increment. Top size is defined as the 95% passing sieve size.
The mass of an increment must be such that it is large enough to include the large particles,
and particles present in the sample should be in the same proportions as in the lot being sam-
pled. The minimum mass of the increment is, therefore, dependent on the size of the particles
being sampled.

Table 1.6: 95% confidence intervals and ranges [10].

Number Low High CV in %

10 0 29.0 98.0
102 4.0 15.0 31.0
103 7.6 11.4 9.8
104 9.2 9.8 3.1
105 9.4 9.6 1.0
106 9.47 9.53 0.3
 Mineral Sampling  15

The top size of a bulk solid is a measure of length. The mass of a particle is a function of its
volume and specific gravity and ultimately a function of its mean diameter or length. The mass
of a primary increment then can be defined in terms of the number and mass of particles from
the top size range. If no other information is available, then an acceptable rule of thumb is to
collect primary increments with a mass equal to 1000 times the mass of a top size particle.

∆M = 1000 ∆M (t ) (1.17)

where
∆M = mass of primary increment in kg
∆M(t) = mass of top size particle in kg
Experience and theory are embodied in a number of national and international standards on
sampling of particulate materials where the sampling regimes are defined in terms of the total
number of increments, and the average mass of a primary increment.
It is generally accepted that a primary increment should contain no less than 1000 particles.
In the standard on sampling of iron ore (ISO TC102), the minimum mass for primary incre-
ments is specified in relation to the top size, and in Table 1.7 these recommendations are
tabulated and compared to calculations for hard coal.
The minimum mass for a primary increment should preferably be defined in terms of the
volume of a particle from the top size range.
Once the mass for a primary increment is selected either in accordance with applicable stan-
dards or on the basis of the previous guidelines, or determined by the critical design param-
eters of a mechanical sampling system, the required number of primary increments remains
to be defined. Too few increments will result in too low a precision, whereas too many would
unnecessarily increase the costs for sampling and preparation.
Most standards for bulk solids contain simple formulae to calculate the required number of
increments for a consignment from a given number for the unit quantity (usually 1000 t), or

Table 1.7: Minimum mass for iron ore and coal primary increments [10].
ISO TC 102 ISO 1988
Top Size (mm) Iron Ore Mass (kg) Hard Coal Mass (kg)

10 0.3 0.6
20 0.8 0.8
50 4 3
100 12 6
150 20 9
250 40 15
16  Chapter 1

Table 1.8: Number of increments to attain a precision of ±0.1 of the true ash [11].
Condition of Coal Conveyors Falling Streams Wagons Barges Seagoing Vessels Stock Piles

Cleaned 16 24 32 32
Uncleaned 32 48 64 64

Table 1.9: Number and mass of increments (ASTM D 2234).

Cleaned Uncleaned
Top Size (mm) Mass (kg) Number Mass (kg) Number

16 1 15 1 35
50 3 15 3 35
150 7 15 7 35

from tables that list the minimum numbers of primary increments as a function of the mass of
a consignment. ISO TC 102 for iron ore specifies this number on the basis of the three levels
of variability which presupposes some knowledge of the expected variability.
Table 1.8 is extracted from ISO 1988 on sampling of hard coal, and lists the number of pri-
mary increments for a 1000 t unit quantity.
Table 1.9 gives the mass and numbers of primary increments for hard coal, as specified in
ASTM D 2234, for consignments of up to 1000 t, and for an estimated precision of ±10% of
the ash content.
For consignments larger than this unit mass of 1000 t, ASTM D 2234 and ISO 1988 use the
same formula to calculate the required number of primary increments:

n = n(t ) ⋅
∑M (1.18)
1000

where
n = required number of increments
M = mass of consignment in tonnes
n(t) = tabulated number of increments
The overall standard deviation of sampling, sample preparation and assay is a function of the
variability of the particulate material, the number and mass of the increments and the random
errors associated with sample preparation and assay. It can be expressed as

σ L2
σ T2 = + σ PA
2
(1.19)
n
 Mineral Sampling  17

where
σL = standard deviation of a primary increment (from Equation (1.3))
σPA = standard deviation of preparation and assay
In a well-balanced sampling regime, the variance of sampling and the variance of preparation
should be of the same order of magnitude.
Dividing a consignment of bulk solids into lots, collecting, preparing and assaying samples
from each lot, and reporting composite assays for the consignment, affects significantly the
precision of the final result. The variance of preparation and analysis may easily become a
limiting factor for the precision of a sampling regime.
If we solve n, the number of primary increments, from the simplified formula for a sampling
regime of only one gross sample per consignment and a single measurement in the final
analysis sample, it follows that [10]

var(d) + var(c) / ∆M
n= (1.20)
var(t) − var(pa)

where
var(c) = composition variance
var(d) = distribution variance
var(pa) = preparation and analysis variance
var(t) = total variance
The denominator of this formula may easily become a limiting factor for the total precision of
sampling regimes since it shows that

n → ∞ for var(pa) → var(t)

Logically, the total variance cannot be smaller than the variance of preparation and analysis.

Example 1.6
Suppose that we have a consignment of 1000 t of iron ore with an assay of 65.0% Fe, and that
we want to determine the assay with a precision of ±10%.
A precision of ±10% of 65.0% Fe is equivalent to ±6.5% of this iron content, and results in a
standard deviation of 6.5/2 = 3.25 for a total variance of 3.252 = 10.56. Substitution of this
total variance of 10.56, composition and distribution variances of, say, 1.66 and 0.71 and an
average mass of 2 kg for primary increments into the formula for n, Equation (1.20), results in

0.71+ 1.66 / 2
n= = 0.146 ~ 1
10.56 − 0.0455
18  Chapter 1

Table 1.10: Precision of sampling regimes and number of increments required [10].
Precision var(t) Lots Increments

±1.0 0.2599 1 8
±0.5 0.0625 1 90
±0.25 0.0156 4 360
±0.25 0.0156 8 155
±0.10 0.0025 32 1430
±0.10 0.0025 64 860

In this case, a sampling regime of one primary increment of 2 kg would result in the required
precision of ±6.5% of the iron content.
For a precision of ±1.0% instead of ±6.5%, how many increments must we collect to attain this
precision?
For an iron assay precision of ±1.0% the standard deviation becomes 1/2 = 0.5 for a total
variance of 0.52 = 0.25. Substitution into Equation (1.20) would result in a number of 7.5 (or
rounded to 8) increments.
If a greater iron assay precision of ±0.25 % is required, then the denominator in the
above equation becomes negative and it is not possible to obtain that degree of
precision sampling from a single lot. The consignment must be divided into sub-lots in
order to determine the assay with this precision. Table 1.10 shows a number of possible
combinations.
These results show that the assay of this particular type of ore cannot be determined with
a precision of ±0.25% at affordable costs because the variance of preparation and analysis
rapidly becomes a limiting factor for the total precision.

In terms of standard deviations, the number of increments may be calculated [1]:

σ L2
n= (1.21)
σ T2 − σ PA
2

When it is impossible to achieve the desired precision by testing a single gross sample from
a lot (e.g. the number of increments is impossibly large), then it is necessary to divide the lot
into a number of sub-lots, nS. Then

σ L2
n= (1.22)
nSσ T2 − σ PA
2

The total number of primary increments for the whole lot then becomes nS × n.
 Mineral Sampling  19

Example 1.7
Calculate the number of increments required in the sampling of silica in iron ore for a desired
overall precision of 0.1, if the increment standard deviation is 1.5 and the preparation and
assay standard deviation is 0.095.

1.52
n= = 2308
0.1 − 0.0952
2

If the lot is divided into, say, eight sub-lots, then

1.52
n= = 32
8(0.1)2 − 0.0952

Therefore, 32 primary increments are required per sub-lot for a total of 8 × 32 = 256 primary
increments in total.

When small amounts of sample are removed from a lot at random and combined to form a
composite sample, the problem is to ascertain the incremental amounts and number of incre-
ments which would represent the bulk within specified limits. Each individual sample will
have an assay equal to, more or less than, the true value. Assuming that a normal Gaussian
distribution will be obtained if the assays were plotted against frequency, the probability that
the assay will be within permissible limits will be given by
X1 x2
2 −  x
P=
π ∫e 2σ 2
d 
σ 
(1.23)
0

where x = deviation from the true assay.

Now if A is the average assay and A1, A2, A3, …, AN are the individual assays of the n sample
increments, then
1
A=
n
( A1 + A2 + A3 +  + An ) (1.24)

and the standard deviation of each increment sample will be

( Ai − A)2
σL = ∑ n
n
(1.25)

The standard deviation of the entire sample, σ, is related to σL by the relation
σL
σ= (1.26)
n
20  Chapter 1

Substituting the values of σ and σL into Equation (1.23) and simplifying gives

h1 h2
2 −
P=
π ∫e 2
dh (1.27)
0

where

KA n x x
h= , K = , then h ≡ (1.28)
σL A σ

The application of this method of estimating n is illustrated in Example 1.8.

Example 1.8
Ten samples were taken from a heap of copper ore each weighing 2 kg. The assays for copper
show the following distribution:

Sample No. 1 2 3 4 5 6 7 8 9 10
Assay 3.0 2.5 2.2 3.2 2.5 2.5 2.3 2.9 3.3 2.1

The final sample should assay within ±5% of the true value with a confidence of 99%. Estimate
the number of increments.

Solution
Step 1
Average assay = (A1 + A2 + A3 +  … + A10)/10 = 2.65
Standard deviation σL = 0.400, from Equation (1.25).

Step 2
For the probability P = 0.99 (given) and using Table 1.4 to simplify the solution of
Equation (1.23),
h = 2.576

Step 3
Calculate the value of h in terms of n where K = 0.05, A = 2.65 and σL = 0.40, from
Equation (1.28)
i.e.

KA n 0.05 × 2.65 n
h= =
σL 0.40
 Mineral Sampling  21

Step 4
2 2
 hσ   2.576 × 0.40 
n= L  = = 60.5
 KA   0.05 × 2.65 

Hence, 61 increments have to be taken whose weight would be 61 × 2 = 122 kg

1.6  Continuous Sampling of Streams

When mechanical samplers are employed, the samplers are designed to cut into and withdraw
from a stream of travelling material at a predetermined frequency and speed. Cutters could
operate linearly or rotate within the stream to be sampled.

1.6.1  Linear Cutters

A schematic design of a linear cutter is illustrated in Figure 1.6. Linear cutters traverse across
the stream to be sampled.
Its operation depends on
• Cutter opening
• Stroke length
• Cutter speed

Figure 1.6: Linear Traversing Sampler.

22  Chapter 1

The rule of thumb for cutter openings is

Normal opening ≅ 3 × largest particle size (dry stream)

Minimum opening ≅ 70 mm for fine particles
≅ 60 mm for fine slurry

It is expected that the opening sizes indicated here would prevent the formation of bridges
across the openings in samplers. Also, the wider the cutter opening the greater could be the
speed of traversing the cutter.
The stroke length is adjusted to cover the width of the conveyer belt where the stream consists
of dry solids, or the width of the stream where liquids or slurries have to be sampled.
The amount of sample (M) cut from any stream by a linear cutter is given by

(Feed rate of stream) (Cutter opening)

M= (1.29)
(Cutter speed)

For a feed rate expressed as kg/s, a cutter speed in m/s and a cutter opening in m, the mass M
is in kilograms. Equation (1.29) can be expressed in terms of volume and written as

(Vol. rate of flow) (Cutter opening)

V= (1.30)
(Cutter speed)

where the unit for volume rate of flow is m3/s, cutter opening, m and cutter speed, m/s.

1.6.2  Rotary Arc Cutter

The rotary type of cutters (Figure 1.7) allows samples to be collected or passed through, as
indicated in the segments. For unbiased sampling, the edge of the cutters equals the radius
of the circle forming the arc. The effective radius, R, swept out by the cutter at any point in
terms of the distance d from the centre of rotation of the cutter to the stream to be sampled
along the centreline is given by
d
R= (1.31)
cos θ

where u is the angle between the radius of the cutter and the centreline of the solids stream.
The cutter opening changes as the cutter moves through the stream; then by simple geometry,
the effective cutter opening, dcutter, at any point is approximately given by
d tan α
Cutter opening, d cutter ≅ (1.32)
cos θ
 Mineral Sampling  23

Figure 1.7: Continuous Rotary Arc Sampler.

If w is the rotational speed (rpm) of the cutter then the cutter speed, Scutter, parallel to the solid
stream can be given by

Scutter = 2π dω cos θ (1.33)

When the leading edge of the cutter reaches the centreline of the discharging conveyor or
stream, cos u = 1; therefore, conditions for dcutter and Scutter reduce to

d cutter = d tan α and Scutter = 2π dω (1.34)

To determine the quantity of sample taken by the arc cutters, it is necessary to know the cut-
ter angle, a. This may be supplied by the manufacturer for a predetermined position of the
cutter or it can be calculated from the following relation:

Cutter arc length

Cutter angle, α = × 360 (1.35)
2π r
24  Chapter 1

The mass of sample of solids, M, recovered per rotation can be computed from a known flow
rate of mineral, MF, by the expression
α MF
M= (1.36)
360ω

MF is expressed in kg/s, and w as rpm.

The volume, V, of liquid or slurry sampled can similarly be written as
α VS
V= (1.37)
360ω
VS is expressed as m3/s.
Note: Usually d = 2/3 radius R of the cutter.

Example 1.9
Dolomite was carried to the bunkers of a blast furnace at the rate of 200 t/h using a 75 cm
wide rubber conveyor belt. The rate of travel of the belt was 61 m/min. The size analysis
of dolomite indicated 95% smaller than 7 cm. The dolomite was sampled as it entered the
bunkers using a linear traversing sampler capable of traversing at the rate of 60 cm/s and
making 20 cuts per hour. Estimate the mass of sample collected in 10 min.
Solution
Step 1
Using rule of thumb, the normal cutter opening = 3 × 0.07 = 0.21 m
Step 2
Using Equation (1.29):
200 × 0.21
Sample mass per cut = = 0.000194 t = 0.194kg
60 × 60 × 60
Step 3
Mass of sample cut in 10 min = 0.194 × 20/6 = 0.647 kg

1.7  Sampling Ores of Precious Metals

Precious metal deposits sometimes contain very low concentrations of discrete metallic par-
ticles as in the case of gold deposits. Extra care is, therefore, needed to collect a representa-
tive sample. If it is assumed that the ore comprises free particles of uniform size, then N, the
number of particles required, is given by

 G
N = 0.45  2  (1.38)
 σS 
 Mineral Sampling  25

where
G = grade of the ore, expressed as volume fraction and
σS = probable error in sampling, expressed as volume fraction
The number of particles per gram, N9, is related to the material density (ρS) and particle size
by an empirical relation as [12]

 6 
N′ =  (1.39)
 ρS d 
3

where
d = limiting screen aperture. This empirical equation covers a range of particle sizes and
shapes.
The mass of sample, M, to be taken can be given as

N  G ρS d 3 
M= = 0.075  (1.40)
N′  σ S 
2

Gy’s method of sampling and determining the minimum mass of sample is also applicable in
this case.
Based on Gy’s method, Eames [13] indicated that the minimum sample required of gold ores
of different particle sizes can be selected from Table 1.11 for normal work.
In developing the table, a 90% confidence level and a relative 15% error have been assumed.
Note: A usual practice is to crush 3.5 kg ore to 95% passing 75 mm sieve size and then taking
a 200 g sample for assay.

Table 1.11: Minimum sample mass for different particle sizes of gold [13].
Au in Mineral (g/t)
Particle Size (mm) 0.01 0.1 1.0 10 30

50 1.45 mt 143 kt 14.3 kt 1.43 kt 477 t

10 11.4 kt 1.14 kt 114 t 11.4 t 3.81 t
5 1.43 kt 143 t 14.3 t 1.43 t 477 kg
1 11.43 t 1.14 t 114 kg 11.4 kg 3.81 kg
0.5 1.42 t 143 kg 14.3 kg 1.43 kg 477 g
0.1 11.4 kg 1.14 kg 114 g 11.4 g 3.81 g
0.05 1.43 kg 143 g 14.3 g 1.43 g 0.48 g
0.01 11.4 kg 1.14 g 0.11 g 0.01 g 3.81 mg
26  Chapter 1

1.8  Sampling Nomographs

When sampling to determine the grade of a large body of material, the sample of 94 kg (for
example) must be reduced to a few grams for chemical analysis. To do this and still maintain
the sampling accuracy, Equation (1.5) suggests that the size of the particles should be reduced
to allow a reduction in the sample mass. To optimise a sampling regime, a sampling nomo-
graph is useful.
A nomograph may be drawn up from theory by rearranging Equation (1.5) to give the
variance (σ2) for a given particle size, dMax as
3
Kd MAX constant
σ2 = = (1.41)
M MIN M MIN

Taking the logs of both sides of Equation (1.41) gives

log σ 2 = constant − log M MIN (1.42)

Therefore, a nomograph plotted on a log–log scale will have a slope of –1, as shown in
Figure 1.8.
The use of the figure is illustrated in the following example. A sample of 94 kg (94,000 g)
is crushed to minus 5 mm and a 30 g sub-sample is split out for gold assay, using a riffle.
The line in Figure 1.8 shows that as the sample mass is reduced, the error associated with a
particle size of 5 mm increases until it exceeds the minimum error specified for this sampling
regime for any sample mass below about 200 g.

Figure 1.8: Sampling Error Vs. Sample Mass-Inappropriate Sampling Regime.

 Mineral Sampling  27

Figure 1.9: More Appropriate Sampling Regime.

To stay within the specified sampling accuracy, a sampling regime similar to Figure 1.9
should be followed.
The 94 kg of minus 5 mm material is sub-divided into a sub-sample mass of 1000 g in the
first stage. This 1 kg of sample is then pulverised to minus 0.5 mm and divided again to
the required sample mass of 30 g. Following this sampling regime will maintain the sampling
procedure below the required sampling error.
To derive a sampling nomograph, Equation (1.5) is used by calculating the sampling constant
K from known data.
An alternative graphical method is to plot sample mass (M) vs. top particle size (dMAX) show-
ing the alternation of size and mass reductions required to maintain an acceptable sampling
variance, governed by the Gy formula (Figure 1.10).
This can be achieved in the following manner:
From Gy’s formula;
3
Kd MAX
M MIN =
σ2

and

log M MIN = (log K − 2 log σ ) + 3 log d MAX (1.43)

28  Chapter 1

Figure 1.10: Alternative Sampling Regime.

Thus for a given value of K and sampling accuracy, this relationship will yield a straight line
of slope 3 when plotted on a log–log graph paper (Figure 1.10). All points on this line (line
BDF, Figure 1.10) have a constant fundamental variance, σ2. The line represents a ‘safety
line’ and splits the graph into two areas.
To the left of this line, the sample mass is greater than the minimum required, MMIN, and the
fundamental sampling variance is less than σ2.
To the right of the line, the sample mass is less than the minimum and the sampling vari-
ance is high and unacceptable. To rectify the situation, either the mass has to be increased or
the particle size, d, has to be decreased to bring the sampling regime back to the left of the
safety line.
A family of lines of equal variance can be constructed, each parallel to one another
(Figure 1.10). From Figure 1.10, for a sample mass of 50 tonnes at a particle size of 9 mm,
and a desired variance of 10−2 or better, the sample can be reduced in mass to 100 kg (A to B)
and still maintain acceptable accuracy (to the left of the safety line). To reduce the mass fur-
ther, the sample must first be reduced in particle size, e.g. to 3 mm (B to C). The sample mass
can then be reduced to 1 g through a sequence of mass reduction and size reduction (C to D to
E to F).

1.9 Problems
1.1 Iron ore was sampled before stock piling with a stacker. One hundred samples taken
from the stacker–conveyor showed a standard deviation in the iron assay of ±0.5%.
The ore assayed, on average, 59% Fe. Sieve analysis of the samples showed that the
 Mineral Sampling  29

largest size was less than 5 mm and the liberation of Fe was maximum in the size
range, −400 + 300 mm. Given that the specific gravity of the ore was 5.3 and the
specific gravity of the gangue was 2.6, estimate the minimum mass of sample required
representing the stack.
1.2 Run-of-Mine iron ore was conveyed on a conveyor belt and sampled at regular intervals.
The sieve analyses and Fe distribution obtained at different sampling frequencies gave the
following results:

Size Range (mm) −6 +5 −5 +4 −4 +3 −3

Mass fraction (%) 10 30 50 10
Fe (%) 61.2 62.0 64.5 62.0

Frequency 20 26 30 40 45 35 8
Fe (%) 54.2 54.0 62.2 64.8 65.5 66.0 67.0

The specific gravity of the ore was 5.5 and that of the gangue material was 2.55.
Determine the minimum mass of sample required to represent the Run-of-Mine ore.
1.3 A pile of gold tailings was augured to sample the dump. A 5 cm diameter drill bit was
used and samples recovered from different depths. The recovered samples were collected
and after mixing thoroughly, the composite was crushed, screened between 125 mm and
75 mm and analysed for gold. The average of 10 gold analyses indicated a value of
200 ± 10 ppm gold. The liberation size of the gold was determined as −43 mm. The
specific gravity of the gold bearing minerals was 4.5 and the associated gangue minerals
were 2.68. Estimate the minimum size of the sample.
1.4 In a metallurgical test, the quality of feed was monitored. Four operators and three
similar test equipment were employed. Material lost in the feed after each operation in
each test was:

Operator
Equipment No. 1 2 3 4
12.5 13.8 12.2 11.5
1 12.8 12.5 12.8 13.1
12.0 13.4 12.1 12.84
12.4 12.8 13.5 13.2
2 11.8 13.0 13.0 12.5
13.2 13.9 12.2 12.8
12.6 12.9 13.2 12.6
3 12.2 12.07 13.0 12.2
13.0 12.7 2.8 13.2

Estimate the variance due to operator and experimental error.

30  Chapter 1

1.5 A mechanical sampler was used to sample a stream of iron ore conveyed on a 1.5 m
wide travelling conveyor at a rate of 90 m/min. and loaded to carry 12 mt/h of ore. The
sample cutter opening was 20 cm square and was operated at a frequency of 5 cuts per
minute. The recovered sample was first crushed to –10 mm and then to –2.5 mm and
analysed for Fe content. The liberation size of Fe was –65 mm and the standard devia-
tion of the Fe content was ±0.15 after the first crushing and the same after the second
crushing. If the average analysis was 59% Fe, estimate
1. The mass of sample cut per minute,
2. The minimum mass of sample required to represent the Fe level of the ore.
1.6 The average assay of a gold sample was 200 ppm Au that varied within 0.5% of the true
assay. 95% of the assays had a probability of 0.99 of the true assay. Specific gravity of
the gold ore was 5.6 and the gangue was 2.54. Determine the size of a crushed gold ore
sample that was taken.
1.7 The mass fractions and distributions of a mixture of sphalerite, chert and middle frac-
tions were determined and the results tabulated below. Compute the size of sample that
should be taken such that its assay may be within 0.2% of the true assay, say 5% with a
probability of 0.99.

Sphalerite Middle Fraction Chert

Mass (%) 0.15 70.85 29.0
Average specific Gravity (ρ) 4.00 2.71 2.65
Average diameter (cm) 2.54 2.54 2.54
Source: Taggart [8,9]

1.8 A gold ore was crushed in a jaw crusher down to 3 mm and to 1 mm in a cone crusher
and finally in a rod mill to minus 75 mm and sampled at each stage. The standard devia-
tion at the first stage was ±10 ppm, ±1 ppm at the second stage and ±0.1 at the third
stage. The confidence level in assaying was 3.0 ± 0.1%. Estimate the minimum mass of
sample to be taken at each stage.
1.9 Three stages of crushing and one stage of riffling were required to get a bauxite ore to
the laboratory for testing. The first stage of crushing produced 100% minus 5 mm, all
products from the second stage passed 2 mm and the product from the third stage of
grinding passed 125 mm. After each stage, the products were sampled and analysed for
alumina. The standard deviations of the alumina determinations were 0.2, 0.1 and 0.05
in the three stages, respectively. The ore assayed 2.1 ± 0.2% of Al2O3.
Estimate the minimum mass of the sample that should be taken to represent the ore after
each stage.
1.10 Ten samples were randomly taken from a 5000 lot of pyrolusite (MnO2) ore. The com-
position and distribution of Mn in each lot was determined. The sampler was designed
 Mineral Sampling  31

to take 5 kg sample at a time. For an assay with a precision of ±1%, estimate the number
of increments required.
Data:
No. 1 2 3 4 5 6 7 8 9 10
Mn (%) 51.8 50.4 49.8 49.0 52.0 53.0 50.0 51.0 50.8 49.9
Wt (%) 78.0 76.8 75.5 77.2 79.0 77.5 76.3 78.3 76.9 79.5

The total standard variance was 0.39.

1.11 A rotary arc cutter sampler was used to cut samples of a mineral conveyed by a con-
veyor belt. The sample cutter was placed 75 cm below the conveyor, which travelled at
a speed of 90 m/min and carried 50 t of the mineral per minute. The maximum cutter
opening was 7 cm.
Estimate:
1. The cutter angle required
2. The quantity of sample taken per cut

References
[1] Draft Australian Standard, DR 00223 2000, Guide to the sampling of particulate materials: part 3 estimating
sampling precision, Standards Australia; 2000.
[2] Allen T. Particle size measurement. 2nd ed. London: Chapman and Hall; 1975.
[3] Heywood H. Trans Instit Chem Eng 1947;25:14.
[4] Irani RR, Callis CF. Particulate size measurement, interpretation and application. New York: John Wiley;
1963.
[5] Lister B. Mining Mag 1980;(Sept.):221.
[6] Guy PM. Int J Mineral Process 1976;3:289.
[7] Guy PM. Sampling of particulate material: theory and practice. Amsterdam: Elsevier Scientific
Publishing Co; 1979.
[8] Wills BA. Mineral processing technology. 4th ed. Oxford: Pergamon Press; 1989.
[9] Taggart AF. Handbook of mineral dressing. London: John Wiley and Sons; 1953.
[10] Merks JW. Sampling and weighing of bulk solids. Clausthal-Zellerfeld: Trans Tech Publications; 1985.
[11] AS 1676–1975, Methods for the sampling of hard coal, Standards Association of Australia; 1975.
[12] Quest and Newell 2002, private communication.
[13] Eames J. Joint seminar by MICA, AIG, Aus. I.M.M. Sydney, 26th July, 1999,81.