Kim Esbensen

Sampling Hall of Fame Sampling Hall of Shame:Illustrating sampling standards with full clarity

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

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

HOW TO write

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), DenmarkPentti Minkkinen Lappeenranta University of Technology (LUT), Finland

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

Alternative title

Agenda

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

2. The work involved in establishing international standards

3. The concept of a HORIZONTAL standard

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

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

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

- and the challenges ..

- a universal sampling standard

Motivation

Many have tried valiantly to infuse TOS into international standards

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 wont 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:

- or just some aspect of TOS principles ...

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.

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.

- THE strategy Accreditation and Quality

Assurance (AQUAL)

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).


Illustration of composite sampling, focusing on using a too small number of

increments, deployed in a too narrow footprint (left), as opposed to a better

composite layout (right).

While improved, sampling is not in compliance with the Fundamental

Sampling Principle (FSP) stipulating that all virtual increments in the lot must

be accessible for physical sampling, which is clearly not the case as the

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.

The continuing fight against superficial 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.

The fight against grab sampling

Principle of Sampling Correctness


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.

The universal fight against grab 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 ...

Sampling Hall of Shame How not to do sampling!

TIATS - BSHGTSI


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). It does not get any better than this ;-)No need for anonymity in such 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 sampling,

Sampling Hall of Shame How NOT TO do sampling

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)

HORIZONTAL: Axiomatic Overview of Theory of Sampling (TOS)

.. aka ..TOS Principle of Preventive Action (PPA)

Normally used in design,

planning, optimization of

a new sampling process

Theory & Practise of Sampling (TOS):

6 Principles and


1. Composite Sampling

2. Particle Size Reduction (comminution)

3. Mixing / blending

4. Representative Mass Reduction (- sample preparation)

Used as active steps in

the sampling process

(often used several

times, in combination)

Theory & Practise of Sampling (TOS):

6 Principles

4 Practical operations

10 Sampling Unit Operations (SUO):10 Sampling Unit Operations (SUO)

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)

7. Composite Sampling

8. Particle Size Reduction (Comminution)

9. Mixing / Blending

10. Representative Mass Reduction


10 Sampling Unit Operations (SUO)

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 SUOs as applied to sampling stages is an inspired contribution from Lars Petersen Julius

HORIZONTAL: Total clarity in description, understanding

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 sampling,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 sampling,

TOS Principle of Preventive Action (PPA)

FSE

GSE

TAE

IDE

IME

IPE

Incorrect sampling Correct sampling

TSE (0-D)

IWE

HORIZONTAL: Implementation strategy (standard revisions)

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

2. CEN proposal (European Standardization Organisation)

3. CEN vs. ISO

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 is (already) out there: AQUAL !!! !!! !!!

8. Only one amendment to local standards is needed:

Strategy for a significantly faster / less laborious implementation:

In the case of conflicting criteria or demands with the present standard ...

HORIZONTAL shall take precedence in all matters regarding sampling

HORIZONTAL

National Taskforce(s)

National Standardisation Committees

International Taskforces

International Standardisation Committees

HORIZONTAL: Dissemination and implementation strategy

National / International Standards / Normgiving documents

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

Your comments are welcome: request the proposal at [email protected]

HORIZONTAL -

a proposal for a matrix-independent standard for representative sampling

Kim H. Esbensen

Francis Pitard

Pentti Minkkinen

Hans S. Mller

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.


Acceditation and Quality Assurrance (AQUAL)

Representative Sampling of Large Kernel Lots (GMO,

contaminants, trace constituents): Variographic Analysis

and Estimation of Total Measurement Uncertainty (3 parts)

Kim H. Esbensen

Pentti Minkkinen

Claudia Paoletti


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

- in press


Representative Sampling - in

Science, Technology and Industry

Esbensen & Minkkinen

Wiley VCH (2012)

Documents

Kim Esbensen