metrological traceability debievre

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      i     n      t     r     o       P       D       B       2       0       0       3     a  Metrological Traceability &  Measurement Uncertainty  Prof Dr P De Bièvre  Independent Consultant  on  Metrology in Chemistry (MiC) IUPAC- Anal Chem Di v Commi ttee WIEN  2004-02-17 ©P De Bièvre WIEN Feb 20 04

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Page 1: Metrological traceability DeBievre

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©P De Bièvre CITAC Sydney Oct1999

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t  r  a  c  e  a  b  i   l   i   t   y  

What istraceability ?

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©P. De BièvreStenungsundNov 1998

Key 1 for Metrology in Chemical Measurement:

Traceability

property of the result of a measurement or the

value of a standard whereby it can be relatedto stated references, usually national or 

international standards, through an unbroken

chain of comparisons all having stateduncertainties

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VIM 1993

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©P De Bièvre Chemand Law Wien Sep 1999

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0.00

0.05

0.10

0.15

0.20

0.25

0.30

0.35

0.40

0.45

0.50

0.55

  c

 

  m  m  o   l  ·   k  g  -   1

-100

-90

-80

-70

-60

-50

-40

-30

-20

-10

0

10

20

   D  e  v   i

  a   t   i  o  n   f  r  o  m   m

   i   d   d   l  e  o   f  c  e  r   t   i   f   i  e   d  r  a  n  g

  e   i  n   %

Experienced laboratory (self-declaration)

Less experienced laboratory (self-declaration)

Non experienced laboratory (self-declaration)

No statement by laboratory

Pb

Results from all participants.

IMEP- 10 : Trace Elements in PolyethyleneCerti fied range [ U =k ·u c (k =2)]: 0.449 - 0.491 mmol·kg

-1

©IMEP CCQM Orlando Feb 1999PORTOROZ Sep 2002

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example of TMU of 15%

around Reference Range

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©P. De Bièvre Sao Paolo Dec 1998

Key 2 for Metrology in Chemical Measurement:

Type A evaluation:method of evaluation of a standarduncertainty by the statistical analysis

of a series of observationsType B evaluation:

method of evaluation of a standard

uncertainty by means other than thestatistical analysis of a series of observations

Uncertainty

ISO BIPM GUM 1993

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©P De Bièvre KASTERLEE Feb 2002RIO de J ANEIRO Apr 2002

EILAT Nov 2003

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Current revision of the VIM:

1. improvement through decrease of - inconsistencies:

•internal within VIM•internal within ISO Guides and Standards

•external between ISO- and non-ISO documents

•no clarity

•no understanding

•no agreement possible

in trade

in implementation of EC Directives

in mutual acceptance of measurement results

- unclarities, since: ...

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©P De Bièvre KASTERLEE Nov 2002EILAT Nov 2003

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The (revision of VIM-2, yielding) VIM-3

2. takes on board chemical measurement

3. uses the “substitution principle”:any definition of a term for the definition of a concept must becapable of replacing that term in another definition

4. uses GUM, even if a number of GUM terms for concepts isalready up for refinement in “GUM-2” (which is not yet planned)

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©P De Bièvre KASTERLEE Nov 2003

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The (revision of VIM-2, yielding) VIM-35. obviously still suffers from a carry-over from 20th - and even19th - century thinking

6. contains “counting quantities is an implicit base quantity”

7. makes uncertainty part of the measurement result8. defines “metrological traceability”9. defines “traceability to the SI”10. defines “measurand” as a “quantity intended for measurement11. includes thinking in terms of “chemical measurement”

(for the first time !)12. includes examples of chemical measurements

(for the first time)13. introduces “calibration hierarchy”14. gives a definition of “comparability”15. specifies any “CRM” as a “measurement standard”

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©PDB KASTERLEE Feb 2003

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Some examples justifying a revision:

example 1: “measurand”

example 2: “measurement result”

example 3: “metrological traceability”

example 4: “measurement uncertainty”

example 5: “measurement unit” and “measurement scale”

example 6: “metrological comparability”

example 7: “target measurement uncertainty”

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Key 2: Measurement uncertainty (MU)

Measure of doubt about the measurement result.

1. an uncertainty of a measurement result is generated automatically

from the very moment one starts measuring

2. measurement uncertainty is obtained through an evaluation process:

- type A evaluation

- type B evaluation

(calculation comes only in at the end, after evaluation)

©P De Bièvre BUCURESTI - MARIBOR - EL QUAHIRA Sep 2001

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3. understanding the process called measurement, is a prerequisite for evaluation of measurement uncertainty

4. measurement uncertainty should be small enough for the intended 

use but, need not be smaller (it can, but need not  be smaller)

©P De Bièvre BUCURESTI - MARIBOR - EL QAHIRA Sep 2001 TALLINN Mar 2002

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©P Taylor GEEL J an 1998

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Uncertainty is new to chemists !

•absent in most university curricula

•ISO/BIPM guide (GUM): only 12 years old !•Repeatability is thought of as uncertainty

•Terra incognita !

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©P. De Bièvre SAPUZ Zürich J uly 1999

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ISO/BIPM-guide:

the new approachre-establishes the responsibility

of the analyst because“evaluation of uncertainty”

is a thinking process !

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©P. De BièvreGeelNov 1992

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DISCREPANCY

PROBLEM NO PROBLEM

DISCREPANCY PROBLEMS CAN BE CAUSED

UNNECESSARILY BY LACK OF

” ORTHODOX” UNCERTAINTY ASSESSMENT

NO DISCREPANCY

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©P De Bièvre KASTERLEE 2004

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©P. De Bièvre Sao Paolo Dec 1998

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Metrology

creates

respect for the law

Lack of Metrology

creates

contempt of the law

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©P De Bièvre SAPUZ ZÜRICH J uly 1999

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The task is

to demonstrate

the authority of the result

of the measurement.

This needs

underpinning (“ Untermauerung” )

of the measurement result

in order to lead tothe necessary credibil ity.

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Key 3: Target Measurement Uncertainty (TMU)

Range of uncertainties from which the analyst claims it contains a

specified “traceable” value for the measurand 

1. The analyst needs a “target” for the measurement uncertainty

he must attempt to achieve

2. A TMU usually originates from a requirement put down byregulatory authorities

©P De Bièvre BUCURESTI - MARIBOR - EL QUAHIRA Sep 2001

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©I SKUBIC PORTOROZ Sep 2002

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TMU

!

   M  e  s  u  r  e  m  e  n   t

  c  o  s   t

increasing QL

increasing TMU

QL

TMUo

MCo

QLo

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©P Taylor GEEL Sep 1999

Metrology in chemistry :The Hubble telescope ...

= the ‘spectacles’ of the analytical chemist

BEFORE AFTER