Challenges of Developing ISO

Sampling Standards
Ralph Holmes
CSIRO Minerals Down Under Flagship
Chair ISO/TC 102/SC 1 Sampling Iron Ore
Chair ISO/TC 27/SC 4 Sampling Coal and Coke
Convenor ISO/TC 183/WG 9 Sampling Cu, Pb, Zn and Ni Concentrates
Introduction
Standards developed by the International Standards Organisation (ISO)
for sampling mineral commodities are criticised for not being adequate
and conforming to Pierre Gys theory of sampling
Is this fully justified?
Always scope for improving ISO sampling standards, but many elements
of the theory of sampling and the requirements for correctly designing
sample cutters are incorporated into current ISO standards for sampling
key mineral commodities, ie, iron ore, coal and coke, and base metals
These standards are continually being reviewed and improved
Difficult task, because they are developed by technical committees on
an international consensus basis
Commercial issues or ignorance can get in the way of correctness
Introduction and adoption of new concepts and procedures takes time
Persistence usually pays off, particularly if changes backed up by hard data
Bad ISO standard are being discontinued, eg, ISO 1988 for coal
ISO Standards Development
Technical Committees established to develop standards for specific
commodities, eg:
ISO/TC 27 (Solid mineral fuels)
ISO/TC 102 (Iron ores)
ISO/TC 183 (Copper, lead, zinc and nickel ores and concentrates)
Sub-committees and Working Groups set up to develop specific
standards for sampling, analysis, physical testing, etc
Countries participating in the development of these standards nominate
representatives to these Sub-committees and Working Groups
Draft standards progress through a number of stages:
Working Draft (WD)
Committee Draft (CD)
Draft International Standard (DIS)
Final Draft International Standard (FDIS)
Publication as an International Standard
Key Requirements for Correct Sampling
The key requirements for ensuring that the samples collected from a
process stream are representative and that the overall precision is
adequate are as follows:
The number of increments taken from the process stream must be sufficient
to obtain the desired sampling and overall precision
All particles in the process stream or stratum must have an equal probability
of being selected and appearing in the final sample for analysis
For a given nominal top size of the material being sampled, there is an
absolute minimum mass of sample that must be retained after division to
control the fundamental sampling error at each sampling stage and obtain
the desired division precision (Gy, 1982)
If these key requirements are incorporated into ISO standards for
sampling mineral commodities, then the standard goes a long way
towards conforming to correct sampling principles and providing
representative samples
Components of Sampling Error
A number of ISO standards developed recently for copper, lead, zinc and
nickel concentrate slurries (ISO 11794) and coal slurries (ISO 20904)
start off by explicitly outlining all the components of the overall sampling
error TSE defined by Gy as follows:
TSE = FE + GE + QE2 + QE3 + WE + DE + EE + PE

where FE = fundamental error

GE = grouping and segregation error
QE2 = long-range quality fluctuation error
QE3 = periodic quality fluctuation error
WE = weighting error
DE = increment delimitation error
EE = increment extraction error
PE = preparation error
The error components are then discussed in detail
Components of Sampling Error
Error components that lead to bias need to be eliminated
Accessory errors
Delimitation and extraction errors
Weighting errors
Others need to be reduced to achieve acceptable precision
Fundamental, grouping and segregation errors
Long-range quality fluctuation error
Periodic quality fluctuation error
Minimising or eliminating bias is critical, because bias cannot be
eliminated once it is present no point in being precisely incorrect
Sources of bias that can be eliminated
Incorrect delimitation and extraction of increments
Sample spillage and contamination
Sources of bias that need to be minimised
Change in moisture content, dust loss, etc
Sampling Precision
Several approaches are used for determining the overall variance in
ISO standards for sampling key mineral commodities
The most comprehensive approach is described in ISO 12743 for
sampling copper, lead, zinc and nickel concentrates, where the overall
variance is expressed as:

sT2 sS2 s 2A

When replicate analyses are carried out:

2 2s 2A
s
T s S
r
In ISO 12743, the sampling variance is broken up into its components
for each sampling stage as follows:
2 2 2 2 s 2A
s T s S1 .... s Si .... s Su 1
r
Sampling Precision
The sampling stage approach is particularly useful for designing and
assessing sampling schemes
To obtain the maximum benefit, the variance between increments for
each sampling stage needs to be determined using the following
equation provided in ISO 12743:
n
(x j x )2
j 1
sb2 2
sPA
i
ni 1
The sampling variance for stage i is then given by:
2
sb2
s Si
i

ni
The overall variance is then given by:
u 1 sb2 s 2A
sT2 i

i 1 ni r
Sampling Precision
The sampling stage approach is a comprehensive approach to
designing a sampling scheme and determining the overall variance,
although quite a lot of work is involved
A simpler approach used in ISO 3082 and ISO 13909-2 for sampling
iron ores and coal and coke respectively is to break up the overall
variance into the primary sampling, sample processing and analytical
variances only as follows:
2 2 2 s 2A
s
T s
S1 s
P
r
The primary sampling variance is determined using a similar process to
that used in the sampling stage method
The sample processing variance is usually determined experimentally
by processing duplicate samples
Sample Cutter Design Requirements
The discharge end of a conveyor is the best location
The cutter must take a complete stream cross-section
The cutting time at each point must be equal
The cutter should intersect the stream in a plane
normal to the stream trajectory
Incorrect
The sample cutter must be non-restrictive, self-
clearing and discharge completely each increment
The plane of the cutter aperture must not be vertical
The cutter aperture must be at least 3d
The cutter speed must be uniform and must not
exceed 0.6 m/s unless the cutter aperture exceeds 3d
Bucket-type cutters must have sufficient capacity
Material from belt scrapers must be sampled
Incorrect
No contamination of the sample or change in quality
Sample Cutter Design
ISO 12743 (Concentrates)
There shall be no impediment to the flow
of concentrate into the cutter at the
maximum flow rate of the concentrate.
The cutter shall be of the self-clearing
type, eg, stainless steel or polythene lined,
discharging each increment completely.
Discharge chute angles shall be a
minimum of 60 to the horizontal.
Correct
No materials other than the concentrate
sample shall be introduced into the cutter,
eg, dust must be prevented from
accumulating in the cutter when in parked
position.
Incorrect - Sample reflux
ISO 3082 (Iron ores)
There shall be no impedance to flow of
sample materials through the sample
cutter at the maximum flow rate.
There shall be no clogging or retention of
residual material in the sample cutter, ie,
the cutter shall be self-clearing.
There shall be no significant change in the
quality of the sample while taking
increments, eg, degradation of the
constituent particles if the sample is taken
for size determination or change in
moisture content if the sample is taken for
moisture determination.
There shall be no contamination or
introduction of material other than the
sample into the sample cutter.
Sample Cutter Design
ISO 12743 (Concentrates)
The cutter shall collect a complete cross-
section of the concentrate stream, both
the leading and trailing edges completely
clearing the stream at the two limits of the
cutter path.
The cutter shall intersect the concentrate
stream either in a plane normal to, or
along an arc normal to, the mean
trajectory of the stream.
Incorrect The cutter shall travel through the
concentrate stream at a uniform speed,
not deviating by more than 5% at any
point.
The geometry of the cutter opening shall
be such that the cutting time at each point
in the stream is equal, not deviating by
more than 5%, ie, straight path cutter shall
have parallel cutter lips and radial cutters
shall have radial cutter lips.
Correct
ISO 3082 (Iron ores)
The sample cutter shall take a complete
cross-section of the ore stream, both the
leading and trailing edges clearing the
stream in one path.
The sample cutter shall intersect the ore
stream either in a plane perpendicular to
or along an arc normal to the mean
trajectory of the stream.
The sample cutter shall travel through the
ore stream at a uniform speed, not
deviating by more than 5% at any point.
The geometry of the cutter aperture shall
be such that the cutting time at each point
in the stream is equal, not deviating by
more than 5%, eg, straight-path cutters
shall have parallel cutter lips and rotary
cutter shall have radial cutter lips.
Sample Cutter Design
Incorrect ISO 12743 (Concentrates)
The cutting aperture of the cutter shall be
not less than 30 mm or, if agglomerates
are present, three times the nominal top
size of the concentrate, whichever is
larger, noting that the cutter aperture may
need to be increased above 30 mm if
blockages occur for wet concentrates.
The maximum cuter speed shall 0.6 m/s
unless the cutter aperture is increased
above the minimum of 3d in accordance
Incorrect with the equation derived by Gy and
Marin.
Bucket cutters shall be of sufficient
capacity to accommodate the increment
mass obtained at the maximum flow rate
of the concentrate.
ISO 3082 (Iron ores)
The cutting aperture of the primary
sampler shall be at least three times the
nominal top size of the ore, or 30 mm,
whichever is the greater. However, with
certain ores, eg, sticky ores, bridging and
consequent bias may occur for a cutter
aperture of three times the nominal top
size. In these instances, larger cutter
apertures shall be used to prevent the
introduction of significant bias.
The maximum cuter speed shall 0.6 m/s
unless the cutter aperture is increased
above the minimum of 3d in accordance
with the equation derived by Gy and
Marin.
Bucket type cutters shall be of sufficient
capacity to accommodate the increment
mass obtained at the maximum flow rate
of ore.
Sampling from Wagons and Stockpiles
Sampling from wagons can only be Correct
conducted if a full vertical column is
extracted
Sampling of stockpiles not permitted

Incorrect Incorrect
Fundamental Error and Minimum Mass
The fundamental error variance 2FE identified by Gy is due to the
particulate nature of the material being sampled and is given by:

2 Cd 3a 2
FE
mS

where C = sampling constant

d = nominal top size (cm)
mS = divided sample mass (g)
a = fractional concentration
The fundamental error leads to the minimum sample mass to achieve
the required precision by transposing the above equation:

Cd3a 2
mS 2
FE
Minimum Sample Mass
The sample mass cannot be reduced below the minimum sample mass
for a given precision until the sample is crushed
This is a critical sampling requirement that must not be ignored if good
division precision is required
While the minimum sample mass can be calculated, it can also be
determined experimentally
Test programs have been conducted by several ISO subcommittees to
establish the minimum sample mass as a function of nominal top size
and required precision as follows:
ISO/TC 27/SC 4 (Sampling coal and coke)
ISO/TC 102/SC 1 (Sampling iron ores)
Minimum Sample Mass
For iron ores (ISO/TC 102/SC 1), a comprehensive international test
work program was conducted, the main contributors being:
Australia, Brazil and Japan
The following equation for minimum sample mass mS (in kilograms) as a
function of division precision D (in % Fe) was subsequently developed
for iron ores based on Gys equation:

0.00032 d2.5
mS
2D

where d = nominal top size (mm)

Incorrect

This equation is included in ISO 3082 for sampling iron ores, which
states clearly that the sample mass cannot be reduced below this
minimum until the sample is crushed
Minimum Sample Mass
Examples of the minimum mass of divided sample for iron ore using
this equation are provided in ISO 3082
Nominal top Minimum mass of divided gross sample (kg)
size (mm) D = 0.1% Fe D = 0.05% Fe
40 325 1,300
31.5 180 710
22.4 75 300
10 10 40
6.3 3.2 13
2.8 0.5 1.7
1.4 0.5 0.5
0.50 0.5 0.5
0.25 0.5 0.5
The masses specified in ISO 3082 are conservative, because the ISO
standard is designed to cover iron ores from around the world
The comparable minimum mass tables for sampling coal are only
partially based on experimental data, but the masses are conservative
System Verification
The latest ISO standards included check lists for
confirming the compliance of sample cutters, including:
Cutter speed
Uniformity of cutter speed while cutting the ore stream
Number of cuts Worn Cutter Aperture
Size and geometry of cutter apertures
Worn and/or missing cutter lips
Build-up and/or blockages in cutter apertures and chutes
Reflux from cutter apertures
Hole in Chute
Ingress of extraneous material when the cutter is parked
Holes in chutes and bins resulting in sample loss Partially Blocked Cutter
Increment/sample mass
Particle size
Conclusion
The principal aspects of the theory of sampling and the requirements for
correctly designing sample cutters have been incorporated into key ISO
standards for sampling mineral commodities, including:
Iron ore
Coal and coke
Copper, lead, zinc and nickel concentrates
These standards play an important part in international trade
However, there is always scope for improvement
Developing new and improving existing standards is not an easy task
Standards are developed by ISO technical committees on a consensus basis
Reaching international consensus is an ongoing challenge
Important for those with a good knowledge of correct sampling practices to
maintain their involvement in ISO committees on a long term basis
Persistence pays off
Dont give up !!
Invitation to Sampling 2012
Date: 21-22 August 2012
Hyatt Hotel, Perth, Australia
Abstracts due by 14 November 2011
Development and application of sampling theory
Drill and blasthole sampling
Plant sampling
Sampling for blending, quality control and metallurgical
accounting
Sampling of commodity exports
New developments in sampling and sample preparation
equipment
Maintenance of sampling equipment and training
Development of national and international standards
Case studies of the application of sampling in
exploration, mining, mineral processing and
environmental monitoring.
http://www.ausimm.com.au/sampling2012/
 ISO/TC 102/SC 1

ISO/TC 102/SC 1 Committee

Thank you
ISO/TC 183