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Sampling Hall of Fame – Sampling Hall of Shame:

Illustrating
HOW TO write sampling standards with full clarity

Kim H. Esbensen National Geological Survey of Denmark and Greenland (GEUS), Denmark
Pentti Minkkinen Lappeenranta University of Technology (LUT), Finland

(with contributions from: Lars Petersen Julius, DONG, Denmark)


Alternative title …

Report on project HORIZONTAL:


WHAT DOES IT TAKE to get full TOS-competence
implemented in International Standards?

Kim H. Esbensen National Geological Survey of Denmark and Greenland (GEUS), Denmark
Pentti Minkkinen Lappeenranta University of Technology (LUT), Finland
(with contributions from: Lars Petersen Julius, DONG, Denmark)
Agenda

1. The role of international standards (analytical, sampling)

2. The work involved in establishing international standards - and the challenges ..

3. The concept of a “HORIZONTAL standard”

4. Design principles: “HORIZONTAL – a matrix-independent sampling standard”


- a universal sampling standard

5. Examples from HORIZONTAL and a coming text-book on sampling

6. Strategy for success re. international standards (national, CEN, ISO)


Motivation
• “Many have tried” – valiantly … to infuse TOS into international standards
- or just some aspect of TOS principles ...
• It is very hard work – it is very frustrating work – it is a continuing uphill battle: WHY?

• The “normal” duration involved in getting a new standard proposed, assessed,


subjected to the required hearings, discussed (fought over) … … 2-3-4 years!

• The chances of succeeding in this endeavor are … … dauntingly small, BECAUSE:


• “More of the same” – won’t work (or, it would have succeeded already, brilliantly)

• A new, alternative strategy is needed … urgently needed, because: there is no time!

• At least: I have no time (nor stomach) for 4+ years of work in (CEN, ISO) committees;
but somebody have to do this, however – and for this purpose ...

• The new strategy is intimately related to HORIZONTAL:


HORIZONTAL: Scope

• HORIZONTAL is a matrix-independent standard for representative sampling.


Compliance with HORIZONTAL is a requirement to claim a specific sampling method
(procedure) as representative.

• HORIZONTAL sets out a minimum competence basis for reliable planning,


performance and assessment of existing, or new sampling procedures with
respect to representativity.

• HORIZONTAL eliminates grab sampling and other incorrect sampling operations, by


requiring conformance with a universal set of seven Sampling Unit Operations.

• HORIZONTAL mandates two simple quality assurance measure, Quality Objectives:


1) sampling of stationary lots, the Relative Sampling Variance test (RSV),
2) sampling of dynamic lots, Variographic Analysis.
HORIZONTAL stipulates maximum threshold levels for QO.
HORIZONTAL: Scope

• HORIZONTAL is based on the Theory of Sampling (TOS). An augmented version of


the HORIZONTAL sampling standard is published separately, and contains all
necessary references and background literature. ”Accreditation and Quality
- THE strategy
Assurance (AQUAL)”
• HORIZONTAL enforces professional self-control by requiring mandatory disclosure of
quality assurance information as produced by RSV or variographic characterisation.

• HORIZONTAL mandates documentation and reporting of sampling representativity


and efficiency for each analyte and class of materials respectively.

• HORIZONTAL employs a dual acceptance approach: items not mentioned herein are
not acceptable as modifications in any sampling procedure or sampling plan, unless
specifically tested and assessed by appropriate QO – while all modifications
successfully passing this test requirement are acceptable.

• HORIZONTAL presents a minimum competency framework for assuming full


professional sampling responsibility.
HORIZONTAL: Total clarity in illustrations (examples)

Neutral illustration focusing on the specific sampling situation (lot, equipment)


only. Distracting elements that could lead to identification related to persons,
buildings, locations, companies have been eliminated, allowing complete focus
on the principal issues, sampling tool (spear) used for grab sampling (right).
HORIZONTAL: Total clarity in illustrations (examples)
The continuing fight against superficial grab sampling

While improved, sampling is not in compliance with the Fundamental


Illustration of composite sampling, focusing on using a too small number of
Sampling Principle (FSP) stipulating that all virtual increments in the lot must
increments, deployed in a too narrow footprint (left), as opposed to a better
be accessible for physical sampling, which is clearly not the case as the
composite layout (right).
spear can only reach the topmost approx. 1 m of the lot. The deeper, major
volume parts of the lot will never be subject to sampling.
HORIZONTAL: Total clarity in illustrations (examples)
The fight against grab sampling

Archetype industrial process sampling – in the form of manual grab sampling.


Uncontrolled IDE and IEE are unavoidable, leading to a significant, inconstant
sampling bias. This type of sampling can never be accepted, on account of
guaranteed non-representativiity.
Principle of Sampling Correctness
HORIZONTAL: Total clarity in illustrations (examples)
The universal fight against grab sampling

The archetype question: optimal size of sampling tool? In some situations there
would appear to be a possible choice of sampling tool sizes (right), while at
others even highly skilled and experienced operators (geologists) may have
difficulties in securing precisely the desired sample volume (right). However:
This is the wrong question being asked at the wrong time.
HORIZONTAL: Total clarity in illustrations (examples)
”Sampling Hall of Shame” – How not to do sampling!

Sampling not in compliance with the Fundamental Sampling Principle (FSP),


must never be accepted, or recommended in international standards. Ditto
for sampling not in accordance with TOS’ Principle of Preventive Action
(PPA) - - allowing IDE, IEE & IPE ...
TIATS - BSHGTSI
HORIZONTAL: Total clarity in illustrations (examples)
”Sampling Hall of Fame” - - - - How to do representative sampling!

Problem-dependent composite sampling par excellence, at Graham Beck


Wines, Franschhoek Valley, South Africa. In order reliably to assess the
state of ripening of wine grapes in an entire plot, the winemaker (left) and
her assistant performs a perfunctory field sampling made up of single
berries from randomly selected vine rows, each sampled at three
alternating height levels, simultaneously alternating between sun-side and
shadow side berries. The final result constitutes a perfect composite
sample, obeying all necessary principles in TOS: vine rows cover the entire
plot; each row is sampled in its entire length comprised by a minimum of 50
grapes; the complete composite sample is macerated, from which a
subsample is produced for rapid sugar determination (employing TOS-
correct mass reduction principles). ItNodoes
neednot
forget any better
anonymity inthan
suchthis … ;-)
examples
HORIZONTAL: Total clarity in illustrations (examples)
”Sampling Hall of Fame” –-- How TO DO representative sampling

Illustration of a TOS-correctly designed vezin cutter, in this case with an


optional number of cutting arms (2,3,4) and exchangeable cutters with
different opening widths, also allowing for easy replacement in the case of
wear and degradation of cutter edges: Excellent design and engineering.

Obvious need for anonymity in such examples


While improved, sampling is still not in compliance with the Fundamental Sampling Principle (FSP) stipulating that all virtual increments in the lot must be accessible for physical s

HORIZONTAL: Total clarity in illustrations (examples)


”Sampling Hall of Shame” – How NOT TO do sampling
HORIZONTAL: Axiomatic Overview of Theory of Sampling (TOS)

1. FSP: Fundamental Sampling Principle


2. SSI: Sampling Scale Invariance
3. .. aka ..TOS’
PSC: Sampling Principle(bias-free
Correctness of Preventive Action (PPA)
sampling)
4. PSS: Sampling Simplicity (primary sampling + mass-reduction)
5. LDT: Lot Dimensionality Transformation
6. LHC: Lot Heterogeneity Characterization (0-D, 1-D)

Theory & Practise of Sampling (TOS): Normally used in design,


planning, optimization of
6 Principles … … … … … … and a new sampling process
HORIZONTAL: Axiomatic Overview of Theory of Sampling (TOS)

1. Composite Sampling
2. Particle Size Reduction (comminution)
3. Mixing / blending
4. Representative Mass Reduction (- sample preparation)

Theory & Practise of Sampling (TOS):

6 Principles … … Used as active steps in


the sampling process
4 Practical operations … …
(often used several
10Sampling
Sampling Unit
Unit Operations
times, in combination)
10 Operations(SUO):
(SUO)
HORIZONTAL: Axiomatic Overview of Theory of Sampling (TOS)

1. FSP: Fundamental Sampling Principle


2. SSI: Sampling Scale Invariance
3. PSC: Sampling Correctness (bias-free sampling)
4. PSS: Sampling Simplicity (primary sampling + mass-reduction)
5. LDT: Lot Dimensionality Transformation
6. LHC: Lot Heterogeneity Characterization (0-D, 1-D)
10 Sampling Unit Operations (SUO)
7. Composite Sampling
8. Particle Size Reduction (Comminution)
9. Mixing / Blending
10. Representative Mass Reduction
HORIZONTAL: Total clarity in expositions (examples …. )
Mission impossible: Overview of TOS in
the format of an international standard

The “tool bar icon” concept of the individual SUO’s as applied to


sampling stages is an inspired contribution from Lars Petersen Julius
While improved, sampling is still not in compliance with the Fundamental Sampling Principle (FSP) stipulating that all virtual increments in the lot must be accessible for physical s

HORIZONTAL: Total clarity in description, understanding …

IDE

FSE

TSE (0-D)
GSE IME

TAE

IPE

IWE

Incorrect sampling Correct sampling

TOS’ Principle of Preventive Action (PPA)


HORIZONTAL: Implementation strategy (standard revisions)

1. DS-XXXX: Horizontal (Danish Standardization Organisation)


2.  CEN proposal … … (European Standardization Organisation)
3. CEN vs. ISO
Strategy for a significantly faster / less laborious implementation:

4. Publication of (augmented) HORIZONTAL in the premier,


peer-reviewed journal: “Accreditation and Quality Control”
5. Committee member do no longer need to fight the very tiresome
battle against trade, commercial, a.o. turf – interests:
7.  HORIZONTAL
” In the case of conflictingiscriteria
(already) out there:
or demands withAQUAL !!! standard
the present !!! !!! ...
Only one amendment
8. HORIZONTAL to “local standards”
shall take precedence is regarding
in all matters needed: sampling”
HORIZONTAL: Dissemination and implementation strategy

HORIZONTAL  National / International Standards / Normgiving documents

National Taskforce(s)

National Standardisation Committees

International Taskforces

International Standardisation Committees

Your comments are welcome: request the proposal at ke@geus.dk

Also: publications in influential peer-reviewed journals in other fora


HORIZONTAL: Dissemination and implementation strategy

HORIZONTAL -
a proposal for a matrix-independent standard for representative sampling

 Acceditation and Quality Assurrance” (AQUAL)

Kim H. Esbensen
Francis Pitard
Pentti Minkkinen
Hans S. Møller
Claudia Paoletti
Lars Petersen Julius

HORIZONTAL is dedicated to Pedro Carrasco, a champion of TOS application in industry and a brilliant proponent of the cause of
representative sampling. In 2010 Pedro tragically lost his battle with cancer during the period where he was chairman planning the 5.th
World Conference on Sampling and Blending (WCSB5). The sampling community mourns his premature passing and misses him greatly.
HORIZONTAL: Dissemination and implementation strategy

Representative Sampling of Large Kernel Lots (GMO,


contaminants, trace constituents): Variographic Analysis
and Estimation of Total Measurement Uncertainty (3- inparts)
press

Kim H. Esbensen
Pentti Minkkinen
Claudia Paoletti

Trends in Analytical Chemistry (TrAC) [2011, 2012]


HORIZONTAL: Dissemination and implementation strategy

”Representative Sampling - in
Science, Technology and Industry”

Esbensen & Minkkinen

Wiley VCH (2012)