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Precision analysis of iron ore sampling, preparation and measurement

overcoming deficiencies in current standard ISO 3085

Article  in  Transactions of the Institution of Mining and Metallurgy, Section A: Mining Technology · June 2011
DOI: 10.1179/1743286311Y.0000000002

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 Precision Analysis of Iron Ore Sampling,
Preparation and Measurement
Overcoming Deficiencies in the Current
Standard ISO 3085
J E Everett1, T J Howard2 and B J Beven3

ABSTRACT
At Cliffs Natural Resources Ltd (CNR) crushing and shipping sample stations, precisions
are estimated for the sampling, preparation and measurement stages of iron ore sampling in
accordance with ISO 3085 (2002). In this Standard, gross duplicate samples are prepared at each
of the three stages, yielding eight measurement assays. Appropriate calculations of the differences
between assay pairs are then made to estimate precision of each stage of sampling.
The International Standard for checking precision in iron ore sampling, ISO 3085 (2002)
prescribes a method for identifying outliers that is ambiguous and possibly inappropriate. The
procedure also makes an unnecessary implicit assumption, that the differences between assay
pairs are normally distributed. The Anderson-Darling statistic is used to demonstrate that in
some cases the assay pair differences have distributions signicantly different from normal. When
applied at CNR as specied, the Standard leads to precision estimates well below the expected
values, thus overestimating the sampling method’’s capability and limiting the opportunity for real
process improvement.
This paper suggests an improved method of estimating sampling, preparation and measurement
precision. A bootstrap procedure is used to estimate condence limits for the calculated precision
estimates. The proposed method would be suitable for testing blasthole precision.
The discussion is supported by extensive simulation modelling of realistic data.

INTRODUCTION
At Cliffs Natural Resources Pty Ltd (CNR) operations at
Koolyanobbing and Esperance in Western Australia, the
precision of the sampling, sample preparation and the
measurement stages of iron ore sampling from the sample
stations at the crusher and port, is estimated placing the
increments alternately into two gross samples (A and B)
which are then processed following Method 1 as outlined in
ISO 3085 (2002).
In processing the data at CNR it was apparent that a literal
application of the standard, which includes an iterative
elimination of outliers, was leading to unrealistically low
estimates for the precision standard errors (particularly
for sampling), thus overestimating the sampling method’’s
capability.
Discussion with practitioners in the iron ore industry
has led the authors to conclude that, for mechanical
sample stations, the ISO 3085 (2002) protocol is generally
interpreted and applied in the same way as is done by CNR.
The overestimating of sampling methods capability is even
greater when the methods are applied to blasthole samples at
CNR. It is recognised that the relevant sampling standard, ISO
3082 (2000), appears to preclude application of the methods
to blasthole samples, as they do not satisfy the condition of
sampling from ‘‘a lot under transfer’’ but, in the absence of
another method, ISO 3085 (2002) is followed in these cases.
CNR management requires realistic values so that
the process capability of each stage of sampling is well
understood and monitored, so that process improvement
effort can be focused on the areas where it is most effective.
This study was requested to clarify what approach CNR
should adopt in processing the sampling precision data to
achieve the above goals.
Three major issues with the ISO 3085 protocol were identied
as leading to the overestimation of process capability:
1. Outliers are identied without adequate statistical
justication, and removed from the data set without
their cause necessarily being removed from the ongoing
operational system.
2. Sampling, preparation and measurement discrepancies are
assumed normally distributed, and unjustied statistical
inferences are made using this implicit assumption.

1. Emeritus Professor of Information Management, School of Business, The University of Western Australia, Nedlands WA 6009. Email: jim.everett@uwa.edu.au
2. MAusIMM, Director, Ore Quality Pty Ltd, PO Box 2579, Warwick WA 6024. Email: orequality@bigpond.com
3. Senior Process Metallurgist, Cliffs Natural Resources Pty Ltd, Koolyanobbing Operations, PMB 8, Southern Cross WA 6426. Email: billie-jo.beven@cliffsnr.com

SAMPLING CONFERENCE / PERTH, WA, 11 - 12 MAY 2010 1

 J E EVERETT, T J HOWARD AND B J BEVEN

3. The sampling, preparation and measurement standard R2(i) = Abs[Xm(i2) - Xm(i1)], for i = 1,2 (4)
deviations are estimated as single values, without any
estimation of their uncertainty. This can lead to clearly
erroneous conclusions, such as zero estimates of the R3 = Abs[X2m(2) - X2m(1)] (5)
standard deviations to cover up calculated negative
estimates. It should be noted that R1, R2 and R3, being absolute values
ISO 3085 (2002) uses the term ‘‘precision’’ both qualitatively of differences between paired values, are each formed from
(such as ‘‘better precision’’) and quantitatively (as ‘‘precision of an equivalent symmetric distribution of zero mean, with the
sampling ǃs’’). The terms ‘‘precision standard deviation’’ and left hand side ipped over to the right hand side, as shown
its square ‘‘precision variance’’ will be used in this paper as in Figure 2. Although Figure 2 shows a normal distribution,
quantitative measures of precision. and ISO 3085 assumes a normal distribution, the actual
distributions of R1, R2 and R3 need not be normal.
BACKGROUND TO THE ISO 3085 STANDARD
PROCEDURE
The ISO 3085 (2002) procedure states a minimum
requirement for the collection of ten, preferably 20, sets (or
‘‘lots’’) of gross duplicate samples. For Method 1, this is done
by:
1. Collecting alternate increments from sample stations
to constitute two gross samples, thereby producing two
equivalent duplicate samples of the same ore (Samples A
and B).
2. Dividing each gross sample into two equal halves, and FIG 2 - The flipped positive distribution and the equivalent symmetric
preparing them separately but equivalently, as A(1), A(2), distribution.
B(1) and B(2).
3. Processing each preparation test sample in duplicate, Since variance is the ‘‘mean squared deviation from the
and measuring their assays equivalently. Two sub- mean’’, it follows that the mean squared values of R1, R2
samples are collected with each sample being beaded and and R3 are the variances of their equivalent symmetric
assayed independently and similarly. This yields eight distributions. Similarly, the mean values of R1, R2 and R3 are
measurement assays named X(111) through X(222) in the the mean absolute values of the symmetric distributions.
Standard. For a normal distribution (as is assumed by ISO 3085), the
Figure 1 summarises the protocol for preparing each lot of mean absolute deviation (MAD) is given by:
eight assays.
MAD = v /Sqrt(Pi/2) = v /1.253 (6)
The assay data are collected for N lots (n = 1, ... N).

Step 1 Step 2a
Equations 1 to 5 show the calculations of paired Xm (the The average values for R1, R2 and R3 are calculated:
mean grades and R1, R2 and R3 (the grade differences) for
each of the N lots. The differences R1, R2 and R3 are absolute R1(ave) = ••nijR1(ij) / 4N (7)
differences between paired values, so all are positive in sign.
The notation here is modied from, but equivalent to, the
notation of ISO 3085 (2002): R2(ave) = ••niR2(i) / 2N (8)

Xm(ij) = [X(ij1) + X(ij2)]/2, for i, j = 1, 2 (1)

R3(ave) = ••nR3 / N (9)

X2m(i) = [Xm(i1) + Xm(i2)]/2, for i = 1,2 (2)

Step 2b
ISO 3085 (2002) species outliers as any R1, R2 or R3 value
R1(ij) = Abs[X(ij2) - X(ij1)] , for i, j = 1, 2 (3) that exceeds 3.267 (‘‘d4’’) times the respective average value.

FIG 1 - Preparing a ‘lot’ of eight assay measurements, following Method 1 of ISO 3085.

2 SAMPLING CONFERENCE / PERTH, WA, 11 - 12 MAY 2010

PRECISION ANALYSIS OF IRON ORE SAMPLING, PREPARATION AND MEASUREMENT
This implicitly assumes all errors are normally distributed, in
which case the root mean square value would be 1.253 times
the mean absolute value, from Equation 6, and the excluded
values would have |z| >2.6, corresponding to p <1 per cent.
(Note that 1.253 × 2.575 = 3.227, and |z| >2.575 corresponds
to p <1 per cent, so the value of 3.267 for d4 is perhaps a
misprint for 3.227).
ISO 3085 (2002) section 7.2.7 states:
When all of the values of R3, R2 and R1 are within the
upper control limits of the R-charts, it is an indication
that the processes of sampling, sample preparation
and measurement of samples are in a state of
statistical control.
On the other hand, when several values of R3, R2 or
R1 fall outside the respective upper control limits, the
process (such as sampling, sample preparation or
measurement) under investigation is not in a state
of statistical control and should be checked in order
to detect assignable causes. Such values should be
excluded and the means of ranges recalculated.
The above instruction is ambiguous, but is commonly
interpreted to imply that steps 2a and 2b should be applied
iteratively until there are no more outliers. It also implies
that there is no need to remove the cause of the outlier, but
just to identify it, even though the cause could reasonably be
expected to repeat itself if not removed.
Discussions with industry practitioners indicate that the
instruction to remove the R value is interpreted in one of two
ways:
Interpretation 1: Any R1, R2 or R3 values outside the
respective upper control limits are eliminated without
considering the implications on other calculated R-values. The
average values and upper control limits are then recalculated,
and the procedure repeated until none of the R1, R2 or R3
values are outside their recalculated upper control limits.
Interpretation 2: Any R1, R2 or R3 values outside the
respective upper control limits are eliminated. If any R1
values have been eliminated, then the R2 and R3 values
whose calculations involve any of the same X values are also
eliminated. If any R2 values have been eliminated, then the
R3 values whose calculations involve any of the same X values
are also eliminated. The respective average values and upper
control limits recalculated, and the procedure repeated until
none of the R1, R2 or R3 values are outside their recalculated
upper control limits.
Interpretation 1 will be used in this paper. Under this
interpretation, any elimination leads to smaller estimates
of the precision variances, for sampling, preparation or
measurement. With Interpretation 2, elimination of R1 values
lying outside the upper control limit will lead to smaller
estimates of measurement standard deviation, but could
change the preparation and sampling standard deviations in
either direction.
Both interpretations, if they are used to eliminate data
without changing the data generating system and collecting
new data, lead to invalid precision estimates, as will be
discussed below.
Step 3a
Let v M2, v P2 and v s2 be the precision variances for
measurement, preparation and sampling, and SM2, SP2 and SS2
be our best estimates of these error variances.
When independent variables are added or subtracted, their
variances add.
SAMPLING CONFERENCE / PERTH, WA, 11 - 12 MAY 2010
Let E[x] denote the expected value of x.
E[R12] = 2v M2 (10)
E[R22] = 2v P2 + (v M2)/2 (11)
E[R32] = 2v S2 + (2v P2)/2 + (2v M2)/4 (12)
On the assumption that all the R-values are normally
distributed, Equation 6 gives:
E[R12] = (1.253*E[R1])2 ; E[R22] = (1.253*E[R2])2; (13)
E[R32] = (1.253*E[R3])2
Our best estimates of E[R1], E[R2] and E[R3] are R1(ave),
R2(ave) and R3(ave), so:
SM2 = (1.253*R1(ave))2/2 = (0.886*R1(ave))2 (14)
SP2 = (0.886*R2(ave))2 - SM2/2 (15)
SS2 = (0.886*R3(ave))2 - SP2/2 - SM2/4 (16)
SSPM2 = SM2 + SP2 + SS2 (17)
Subtracting the calculated variances of the higher levels
of measurement and preparation error compounds the
uncertainty in the sampling variance, which is the last one
calculated. Because the sample variance estimates (SS2)
are estimates of a population variance, calculated from a
relatively small number of data points subject to random
error, they can turn out to be negative. Since we know the
population variances (v 2) they are estimating cannot be
negative, the protocol replaces any negative estimates by zero.
As will be discussed later, the method provides only a single
point estimate of each s2 statistic, and a zero estimate should
not be expressed as a precision variance of zero but should
more validly be expressed as ‘‘greater than zero’’, or essentially
‘‘indeterminate’’.
Step 3b
Again assuming errors are normally distributed, there is about
a ve per cent chance an error will exceed plus or minus two
standard deviations. So the 95 per cent ± precision ranges b M,
b P, b S and b SPM are estimated as:
b M = 2SM ; b P = 2SP ; b S = 2SS ; b SPM = 2SSPM (18)
ISSUES WITH THE ISO 3085 PROTOCOL
The three major issues with the ISO 3085 procedure are:
Issue 1: Large values of R1, R2 or R3 can be identied as
outliers (based on the normal distribution assumption), and
eliminated. If the distribution is not normal (see Issue 2), or if
the number of lots is reasonably large, discrepancies outside
the upper control limits may not really be outliers but part
of the process. Whether they are outliers or not, eliminating
such values without eliminating their cause will tend to
underestimate the precision variances.
Issue 2: The sampling, preparation and measurement
discrepancies, whose variances are to be estimated, are
3
 J E EVERETT, T J HOWARD AND B J BEVEN

assumed normally distributed. If the distributions are not
normal, then using the mean absolute deviations of R1, R2
and R3 to estimate the precision variances is not statistically
valid.
Issue 3: The protocol provides only single estimates of the
precision variances. Since the estimates are based on a nite
range of data, they will themselves have uncertainties that are
not estimated by the protocol. This deciency is particularly
serious when a negative sample variance is replaced by a zero
value, when we know the true population parameter has to be
larger than zero.
These three issues will be discussed in detail, and an
alternative approach recommended for overcoming the issues.
The identification and elimination of outliers
In step 2 of the ISO 3085 protocol, outliers are eliminated if
they exceed a threshold value; the computation is repeated
excluding them, and the procedure is repeated until no
outliers are evident.
This would be justiable if the sampling systems were
examined, the cause of the anomalous value identied, and
that cause eliminated from future data gathering. For example,
if every outlier could be related to data from a faulty machine
in the laboratory that produced intermittent errors, and the
faulty machine repaired, the outliers could then justiably be
eliminated.
If the underlying cause of the outliers has not been identied
and eliminated, then whatever caused them has the potential
to recur in future work. Estimating error variances from the
data after eliminating outliers, without eliminating their cause,
will therefore under estimate the true precision variance and
over estimate the sampling process capability.
Table 1 shows a real example, using CNR port lump Fe
precision testing data to illustrate the effect on precision
estimates of removing outliers. The outlier elimination
method has followed ‘‘Interpretation 1’’, as described above.
Each iteration step removes outliers, reducing the average
R-values and thus the thresholds for elimination. This can
make new outliers appear. In the example it takes three
iterations to eliminate all seven outliers, four per cent of the
175 original R-values. The measurement precision standard
deviation is reduced by 29 per cent, the others by rather less.
Table 2 shows the results for LOI, for the same data set. In
this case four iterations are required to remove 13 outliers. The
measurement precision standard deviation is nearly halved.
One potentially invalid reason for considering and
eliminating outliers is the assumption that the errors are
normally distributed. The next section will show that the R1,
R2 and R3 values are not necessarily distributed normally.
Even if they did have normal distributions, the protocol would
reject as outliers any values outside the 99 per cent condence
limits. If, as in the example of Table 1, the analysis is based
on 25 lots, then there are 100 R1, 50 R2 and 25 R3 values. Of
the total 175 R-values, an average of nearly two values would
be expected to lie above the 99 per cent condence limit, even
for a system under statistical control. The probability of no
such ‘‘outliers’’ is the probability of a 99 per cent chance being
repeated 175 times, and is therefore only 17 per cent (= 0.99175).
The assumption of a normal distribution for
difference values R1, R2 and R3
In many situations, it is reasonable to assume a normal
distribution. This is because of the ‘‘Central Limit Theorem’’
which tells us that if we add or subtract several distributions
of comparable and independent variance, the resulting
distribution will rapidly approach a normal distribution. So,
for example, we can assume a normal distribution for the
error in the estimate of the grade for a day’’s production, if the
estimate is the average from a number of samples taken from
uniform tonnages through the day.
Our precision data cannot be assumed to follow a normal
distribution, as each discrepancy may have only a single
cause. If there are multiple causes they may be of differing
magnitude, or compounded by multiplication instead of
addition. For example, in the situation where two successive
stages of analysis each contribute error, the cumulative effect
can be multiplicative. In this case, the Central Limit Theorem
would give rise to a log normal distribution. Alternatively, the
discrepancies may be from two distinct populations, so that
the underlying distribution is bimodal. Either situation will
lead to the discrepancies not being normally distributed.

TABLE 1
Iterative elimination of outliers from Fe data set (contains 25 lots).

Iter R1 R2 R3 Measure Prepare Sample Total Measure Prepare Sample Total

Step (ave) (ave) (ave) s(M) s(P) s(S) s(SPM) Data Out Data Out Data Out Data Out
1 .060 .200 .255 .053 .173 .188 .313 100 4 50 1 25 1 175 6
2 .044 .191 .230 .039 .167 .165 .287 96 1 49 24 169 1
3 .043 .191 .230 .038 .167 .165 .287 95 49 24 168 0

TABLE 2
Iterative elimination of outliers from LOI data set (contains 25 lots).

Iter R1 R2 R3 Measure Prepare Sample Total Measure Prepare Sample Total

Step (ave) (ave) (ave) s(M) s(P) s(S) s(SPM) Data Out Data Out Data Out Data Out
1 .059 .106 .119 .052 .086 .082 .156 100 4 50 2 25 175 6
2 .037 .091 .119 .033 .077 .089 .145 96 5 48 1 25 169 6
3 .031 .086 .119 .028 .073 .091 .142 91 47 1 25 163 1
4 .031 .081 .119 .028 .069 .092 .140 91 46 25 162 0

4 SAMPLING CONFERENCE / PERTH, WA, 11 - 12 MAY 2010

PRECISION ANALYSIS OF IRON ORE SAMPLING, PREPARATION AND MEASUREMENT
If the errors were normally distributed, then the distributions
of R1, R2 and R3 (being absolute differences) would each be
the right-hand side of a normal distribution of zero mean.
Figure 3 shows the distributions of R1, R2 and R3, for the
same 25-lot lump Fe data set of Table 1. It is clear that R1 is not
normally distributed, even if R2 and R3 may be. The dots are
the actual values. The solid lines each represent the ‘‘ipped’’
normal distribution that has the same root mean square value
as the actual values.
There are statistical methods to test whether a distribution
is signicantly different from normal.
The Kolmogorov-Smirnov distribution is often used as a test
for normality, but should not be used unless the parameters of
the normal distribution are exogenous, not generated by the
data, as is the case in our data set. For example, it can be used
to test if data matches a normal distribution of given mean
zero and standard deviation, parameters based on some prior
hypothesis, but only if these mean and standard deviation
parameters are not sample statistics taken from the data being
tested.
The Anderson-Darling A2 statistic provides a test that does
not suffer from this restriction and therefore is suitable to test
our data. A good discussion is found in Wikipedia (2009) and
the source references (Anderson and Darling, 1952; Stephens,
1974).
Anderson-Darling test for normality
To test for a normal distribution, the data {Xn, n = 1, 2 ... N}
are rst standardised to values Yn by subtracting the mean XM
and dividing by the standard deviation sX.
Yn = (Xn - XM)/sX (19)
FIG 3 - Distributions of R1, R2 and R3 values for Fe data.
TABLE 3
Anderson-Darling test for normal distribution.
Test for Normal Distribution
(A*2 = Anderson-Darling Statistic)
R1
A*2
11.433
Result Reject p <1%
SAMPLING CONFERENCE / PERTH, WA, 11 - 12 MAY 2010
From the cumulative normal distribution function U(Yn),
the statistic A2 is now calculated:
A2 = -N - (1/N)*••n[(2n-1)ln U(Yn) + (2(N-n) (20)
+1)ln(1- U(Yn))]
The value of A2 is modied to A*2 by an approximate
adjustment for sample size J:
A*2 = A2(1+4/J-25/J2) (21)
Generally N and J would be equal, and equal to the number
of observations.
But in our study, we are testing the half-distribution R (R1,
R2 or R3). So the R distribution has to be reected into the
negative region, creating double the data points, with zero
mean and standard deviation equal to the root mean square
of R*. N is thus equal to eight times the number of lots when
testing R1, four times the number of lots when testing R2, and
twice the number of lots when testing R3. J, the number of
actual observations, is in each case half the value of N, because
of the ‘‘ipping’’ nature of the R-distributions.
The values of A*2 to reject the null hypothesis of normality are
given in the literature as (0.632, 0.751, 1.029) for signicance
levels of (ten per cent, ve per cent, one per cent).
Table 3 shows the results for the Fe data set of Figure 3. R1 has
an Anderson-Darling statistic of 11.433. This is much bigger
than the one per cent signicance level, so we can condently
reject the hypothesis that, in this data set, R1 follows a normal
distribution.
The Anderson-Darling statistics for R2 and R3, 0.281 and
0.280 are both well below the ten per cent signicance level of
R2 R3
0.281 0.280
Accept Normal Accept Normal
5

0.632. The hypothesis that they are from normal distributions
can therefore be accepted, in both cases. The failure to reject
the normal distribution for R2 and R3 does not prove they are
normal distributions. With other sets of CNR precision testing
data, the test has often shown R2 and/or R3 fail the normality
test. For example, the LOI data set of Table 2 gives Anderson-
Darling statistics of (23.45, 1.118, 0.179) for R1, R2, R3), so in
this case normality is rejected for R1 and R2, but not R3.
Consequences of non-normality
The conclusion that the precision errors do not necessarily
have a normal distribution negates much of the procedure for
ISO 3085 (2002), particularly in step 2 described above.
ISO 3085 (2002) implicitly uses the average values of R1, R2
and R3 to predict their root mean square values, applying a
factor of 1.253. This is valid only if the underlying distribution
is normal. It is also unnecessary, because the root mean
square values are easily calculable. The use of mean absolute
values is perhaps a relic from the days before easily accessible
computing power.
The identication and elimination of outliers also stems from
the normal distribution assumption. If the assumption were
true, very few values would lie outside the outlier threshold.
Given the assumption of normality is not warranted more
values could lie outside the outlier threshold, so iteratively
eliminating such values can distort the results by even more,
as we have seen in Table 1 and Table 2.
The non-normality of the distributions does not affect the
parts of the standard that depend upon the cumulation of
variance when independent variables are added or subtracted,
as in Equations 10 to 12. For two independent variables X and
Y, with variance v X2 and v Y2, the following relationship is
true, whatever the distributions of X and Y:
v X+Y2 = v X2 + v Y2 (22)
Equations 10 to 12 all derive from Equation 22, and do not
depend upon the assumption of normality.
Single estimates versus confidence limits
Since the error distributions may not be normal, the precision
ranges b M, b P, b S and b SPM of Equation 17 do not represent
95 per cent condence limits for individual assay
measurements, in the precision calculation case. However,
if we were taking the mean of a number of measurements,
such as assays taken each kilotonne for an ‘‘n’’ kilotonne
batch, to estimate the grade of the total batch, then ! b SPM/
n0.5 will represent the 95 per cent condence limits, because
the central limit theorem will ensure that the (independent)
assays will average out to an (almost) normal distribution.
But there remains a problem that throws further doubt
on the condence limits. The s values, from which the b
values are derived, are themselves estimates of an unknown
parameter v . This parameter estimate itself has uncertainty,
whose magnitude is inversely related to the number of lots
used in the precision analysis. The proposed revision of
the ISO 3085 procedure therefore includes a bootstrap
procedure to establish condence limits on our estimates SM,
SP, SS and SSPM.
PROPOSED PROCEDURE TO ADDRESS
THE ISSUES
To address the issues identied in ISO 3085 (2002), we
suggest the following modications to its procedural steps.
6 SAMPLING CONFERENCE / PERTH, WA, 11 - 12 MAY 2010
J E EVERETT, T J HOWARD AND B J BEVEN
Step 1
This step in the calculations does not need changing.
Step 2
The root mean square values for R1, R2 and R3 should be
calculated, instead of the mean values.
R1(rms) = Sqrt[••nijR1(ij)2/4N] (23)
R2(rms) = Sqrt[••niR2(i)2/2N] (24)
R3(rms) = Sqrt[••nR32/N] (25)
No extreme values should be eliminated as outliers, unless
some operational cause for variation has been identied and
eliminated (for example, extremely large values might be
investigated to see if some identiable cause was associated
with their occurrence). To ensure that such elimination
is valid, a new set of data would need to be collected and
processed, with the operational cause of variation eliminated.
Step 3
The error variances for measurement, preparation and
sampling, can now be estimated:
SM2 = R1(rms)2/2 (26)
SP2 = R2(rms)2/2 - SM2/2 (27)
SS2 = R3(rms)2/2 - Sp2/2 - SM2/4 (28)
SSPM2 = SM2 + SP2 + SS2 (29)
Because we cannot assume errors are normally distributed,
we cannot double the estimated standard errors, as in
Equation 18, and use them as 95 per cent condence ranges.
However, we can use a bootstrapping method to estimate
the condence ranges of the error variances SM2, SP2, SS2 and
SSPM2. This method will be described in the next section. It
should be emphasised that the bootstrapping method to be
described provides condence limits for the parameters v M2,
v P2, v S2 and v SPM2, not condence limits for individual errors,
as b M, b P, b S and b SPM were intended to do.
Comparison of the procedures
Table 4 compares the results obtained using the ISO 3085
method (using Interpretation 1 for removing outliers) with
those from the proposed ‘‘RMS’’ method, using the same 25 lot
data set, PLS Fe data from the Esperance shipping sample
station.
The ISO 3085 results are the rst and last iterations from
Table 1. The RMS measurement precision standard errors
deviation is somewhat larger than that from even the rst,
ISO 3085 iteration, prior to the removal of any outliers.
The variances estimated by the proposed RMS procedure are
efcient and unbiased estimates of the population parameters.
However, they are only estimates, based upon nite data, and
will themselves contain uncertainties. These uncertainties will
be expected to relate inversely to the number of lots used in
the precision analysis.
PRECISION ANALYSIS OF IRON ORE SAMPLING, PREPARATION AND MEASUREMENT

TABLE 4
Comparison of the ISO 3085 and the proposed ‘RMS’ procedures.

Iteration Step Measure R1(ave) Prepare R2(ave) Sample R3(ave) Measure s(M) Prepare s(P) Sample s(S) Total s(SPM)
1 .060 .200 .255 .053 .173 .188 .313
2 .044 .191 .230 .039 .167 .165 .287
3 .043 .191 .230 .038 .167 .165 .287
RMS Method R1(rms) R2(rms) R3(rms) s(M) s(P) s(S) s(SPM)
.105 .260 .316 .074 .176 .182 .264
A bootstrap procedure is proposed for estimating the extraction of many samples (typically 1000 samples), each of
uncertainty in the precision estimates. This bootstrap procedure M items, sampling with replacement, so any one value may
will be discussed in the next section. be picked none, one or multiple times within a single sample.
The parameter of interest is then estimated from each sample.
Bootstrapping confidence limits for the For N lots, M is 4N for R1; 2N for R2, and equal to N for R3.
precision variance This method has been applied to the same CNR Fe data.
The error variance estimates SM2, SP2, SS2 and SSPM2 have a From the 25 lots, we have populations of 100 R1 values,
degree of uncertainty which in turn can be estimated by 50 R2 values and 25 R3 values. One thousand simulations are
bootstrapping methods (see for example, Chernick, 2008). run, each extracting a sample of 100 R1 values, 50 R2 values
There are a number of bootstrapping methods available, but and 25 R3 values, sampling from the populations at random,
the ‘‘Case Resampling’’ approach is a parameter-free method, with replacement. Each sample from these populations is
then subjected to the proposed procedure, described above,
which is appropriate, since we do not know the underlying
to estimate R1(rms), R2(rms) and R3(rms). From these, SM2,
distribution. As we have seen, we cannot assume it is a normal
SP2, SS2 and SSPM2 are recalculated according to Equations 22
distribution.
to 28. The probability distributions resulting from the 1000
In the discussion that follows, ‘‘sample’’ is being used in a simulations are tabulated in Table 5. The ‘‘best estimate’’ is that
statistical sense, and is not to be confused with the original for the original 25 lot data set, specically the ‘‘RMS’’ method
metallurgical data set. results noted in Table 5. The bootstrap results show that the
In Case Resampling, the R1, R2 and R3 values are each precision estimates contain considerable uncertainty. The
treated as a population, from which we take samples of the upper 95 per cent condence limits show that the population
same size. To do this, we take our set of M data values, assign parameter may well be much greater than our best estimate.
them equal probabilities (equal to 1/M), and then simulate the And it should be remembered that this is the uncertainty in

TABLE 5
Bootstrap parameter estimate distributions.

Bootstrap percentile Measure s(M) Prepare s(P) Sample s(S) Total s(SPM)
0% .032 .107 .000 .191
1% .041 .125 .071 .206
2% .043 .131 .083 .211
5% .048 .143 .103 .219
10% .054 .150 .124 .229
20% .061 .160 .140 .238
30% .066 .166 .153 .246
40% .069 .172 .163 .252
50% .073 .176 .174 .258
60% .077 .180 .185 .267
70% .080 .185 .198 .277
80% .085 .191 .214 .286
90% .090 .200 .232 .299
95% .096 .207 .244 .311
98% .102 .214 .259 .324
99% .105 .218 .269 .334
100% .113 .228 .308 .357
RMS Method .074 .176 .182 .264

SAMPLING CONFERENCE / PERTH, WA, 11 - 12 MAY 2010 7

 J E EVERETT, T J HOWARD AND B J BEVEN

the parameter itself, the standard error. Individual errors
may be two or more times the standard error. The only way
to extract tighter precision estimates is to analyse more lots.
The bootstrap results are graphed in Figure 4. The horizontal
bars show the ‘‘standard error of the precision estimates’’.
BLASTHOLE SAMPLES
ISO 3085 (2002) species that sampling be carried out
in accordance with ISO 3082 (2000), which requires that
samples be taken from a lot under transfer. This would appear
to preclude using the methods of ISO 3085 for samples
taken from blastholes, where the assumption of normal
distributions would be even more dubious, and where the
large error variance of sampling precision is likely to swamp
the estimates of preparation and measurement precision.
However, the methods suggested in this paper do not require
the assumption that R1, R2 and R3 are normally distributed,
which means that they could be applied to samples taken from
blastholes.
For blasthole sampling, two radial cuts are collected from
the blast cone at 90° apart (Sample A) and duplicated at 45° to
the original (Sample B). The samples collected are processed
following Method 1 as outlined in ISO 3085 (2002).
Table 6 shows the results from applying the ISO 3085
method to 20 lots of blasthole Fe sample data from
Koolyanobbing. In this example, it takes eight iterations to
eliminate all 15 outliers, totalling nearly 11 per cent of the
140 original R-values. The precision standard deviation
estimates for sampling s(S) and preparation s(P) are reduced
to a small fraction of their initial values whereas the precision
standard deviation for measurement s(M) remains relatively
unaffected.
The R-values are plotted in Figure 5, and the results for the
Anderson-Darling test for normality are reported in Table 7.
For these blasthole data, R1 values can be taken as normally
distributed, but the R2 and R3 values cannot.
Table 8 compares the ISO 3085 and RMS precision
estimates. The RMS estimates are larger than, but comparable
to, the rst ISO 3085 iteration, but the last iteration, as we
have seen, gives much smaller estimates of the preparation
and sampling standard errors, with the sampling standard
errors being much smaller than anticipated for blasthole data.
Bootstrap analysis provided estimates of the probability
distributions for the precision standard deviations, as shown
in Figure 6. The sampling precision standard deviation is
much bigger than the other two precisions, as would be
expected for blasthole data.

Cumulative
Probability
100%

90%

80%

70%

60%

50%

40%
Measure s(M)

30% Prepare s(P)

Sample s(S)
20%
Total s(SPM)

10%
Standard Deviation
0%
0 0.05 0.1 0.15 0.2 0.25 0.3

FIG 4 - Bootstrap parameter estimate distributions.

TABLE 6
Iterative outlier elimination for Fe blasthole data (20 lots).

Iter R1 R2 R3 Measure Prepare Sample Total Measure Prepare Sample Total

Step (ave) (ave) (ave) s(M) s(P) s(S) s(SPM) Data Out Data Out Data Out Data Out
1 .049 .200 .647 .043 .174 .559 .671 80 1 40 3 20 1 140 5
2 .046 .099 .505 .041 .083 .443 .513 79 37 3 19 1 135 4
3 .046 .073 .417 .041 .057 .367 .423 79 34 18 1 131 1
4 .046 .073 .349 .041 .057 .306 .356 79 34 17 1 130 1
5 .046 .073 .297 .041 .057 .260 .306 79 34 16 1 129 1
6 .046 .073 .246 .041 .057 .213 .256 79 34 15 1 128 1
7 .046 .073 .206 .041 .057 .177 .217 79 34 14 2 127 2
8 .046 .073 .121 .041 .057 .097 .140 79 34 12 125 0

8 SAMPLING CONFERENCE / PERTH, WA, 11 - 12 MAY 2010

PRECISION ANALYSIS OF IRON ORE SAMPLING, PREPARATION AND MEASUREMENT

TABLE 7
Test for normal distribution (blasthole data).

Test for Normal Distribution

(A*2 = Anderson-Darling Statistic)
R1 R2 R3
A*2 0.615 10.990 2.197
Result Accept Normal Reject p <1% Reject p <1%

TABLE 8
Comparison of ISO and RMS estimates for blasthole Fe data.

Iteration Step Measure R1(ave) Prepare R2(ave) Sample R3(ave) Measure s(M) Prepare s(P) Sample s(S) Total s(SPM)
1 .049 .200 .647 .043 .174 .559 .671
... ... ... ... ... ... ... ...
8 .046 .073 .121 .041 .057 .097 .140
RMS Method R1(rms) R2(rms) R3(rms) s(M) s(P) s(S) s(SPM)
.064 .420 1.060 .045 .295 .719 .779

Cumulative
Probability
100%

90%

80%

70%

60%

50%

40%

30% R1 Observed Fitted Normal

R2 Observed Fitted Normal
20% R3 Observed Fitted Normal

10%
R-Value
0%
0 0.5 1 1.5 2 2.5 3

FIG 5 - Distributions of R1, R2 and R3 values, Fe blasthole data.

Cumulative
Probability
100%

90%

80%

70%

60%

50%

40%
Measure s(M)
30% Prepare s(P)

20% Sample s(S)

Total s(SPM)
10%
Standard Deviation
0%
0 0.2 0.4 0.6 0.8 1

FIG 6 - Bootstrap parameter estimate distributions for Fe blasthole data.

SAMPLING CONFERENCE / PERTH, WA, 11 - 12 MAY 2010 9


CONCLUSION
This study has considered some issues with the current ISO
3085 protocol for estimating sampling, preparation and
measurement previsions. Deciencies arise from an implicit
but unwarranted assumption that individual precisions are
normally distributed. The method also has an ambiguous
procedure for the elimination of outliers from the analysis.
The specied procedure in ISO 3085 is ambiguous as
generally interpreted, and can lead to the elimination of
outliers, even if their cause has not been identied and
removed from the operational system.
It has been shown that we cannot assume the distributions
are normal. A revised procedure has been proposed, avoiding
the normal distribution assumptions, and a bootstrapping
method applied to estimate the uncertainties in the estimates
of sampling, preparation and measurement precisions. An
Excel program, using Visual Basic macros (VBA applies the
methods discussed in this report, to carry out the proposed
precision analysis procedure and, for comparison, the iterative
ISO 3085 procedure.
It is suggested that, being free of the normality assumptions
and outlier categorisation, the ‘‘RMS’’ method described may
be suitable for blasthole samples as well as for ‘‘lots under
transfer’’ as specied in ISO 3082 (2000).
10
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J E EVERETT, T J HOWARD AND B J BEVEN
ACKNOWLEDGEMENTS
The authors wish to thank the management of Cliffs Natural
Resources Pty Ltd for permission to publish this manuscript.
REFERENCES
Anderson, T W and Darling, D A, 1952. Asymptotic theory of certain
‘‘goodness-of-t’’ criteria based on stochastic processes, Annals of
Mathematical Statistics, 23:193-212.
Chernick, M R, 2008. Bootstrap Methods: A Practitioner’’s Guide,
second edition, Wiley Series in Probability and Statistics, (Wiley:
New Jersey).
ISO 3082, 2000. Iron Ores –– Sampling and Sample Preparation
Procedures, third Edition, International Standards (SAI Global:
Sydney).
ISO 3085, 2002. Iron Ores –– Experimental Methods for Checking the
Precision of Sampling, Sample Preparation and Measurement,
fourth Edition, International Standards (SAI Global: Sydney).
Stephens, M A, 1974. EDF statistics for goodness of t and some
comparisons, Journal of the American Statistical Association,
69:730-737.
Wikipedia, 2009. Anderson––Darling test [online]. Available from:
<http://en.wikipedia.org/wiki/Anderson%E2%80%93Darling_
test>.
SAMPLING CONFERENCE / PERTH, WA, 11 - 12 MAY 2010