qualimetry in spectrochemical...
TRANSCRIPT
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QUALIMETRY IN
SPECTROCHEMICAL
ANALYSIS
Quality control on analytical laboratory
V. KmetovUniversity of Plovdiv, BULGARIA
EuRopean Community Action Scheme for the Mobility of University Students)
Academic exchange
University of Alicante,
March 2015
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Slide 2V. Kmetov, Alicante 2015
LONG AND FRUITFUL PARTNERSHIP
TEMPUS S_JEP12451-97
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Slide 3V. Kmetov, Alicante 2015
LONG AND FRUITFUL PARTNERSHIP
ERASMUS MOBILITY
Plovdiv –> Alicante - 24 Students
Alicante -> Plovdiv – 2 Student
Alicante –> Plovdiv - 7 professors + 2 admin.
Plovdiv –> Alicante - 7 professors + 1 Rector
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Slide 4V. Kmetov, Alicante 2015
GGGreen
AAAnalytical
MMMethods
AAAcademic Centre
http://gama.argon.uni-plovdiv.bg/
National Science Found of Bulgaria
INTIGRATED RESEARCH CENTRES AT THE
UNIVERSITIES
UNIVERSITY CENTRE FOR DEVELOPMENT OF
GREEN CHEMISTRY METHODS FOR TRACE
ANALYSIS OF ENVIRONMENTAL OBJECTS
LONG AND FRUITFUL PARTNERSHIP
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Slide 5V. Kmetov, Alicante 2015
Prof. Dr. Antonio Canals – DOCTOR HONORIS CAUSA
OF THE UNIVESRITY OF PLOVDIV “Paisii Hilendarski”
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Slide 6V. Kmetov, Alicante 2015
QUALIMETRY IN
SPECTROCHEMICAL
ANALYSIS
Quality control on analytical laboratory
V. KmetovUniversity of Plovdiv, BULGARIA
EuRopean Community Action Scheme for the Mobility of University Students)
Academic exchange
University of Alicante,
March 2015
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Slide 7V. Kmetov, Alicante 2015
1.The new trends in the global economy and
the needs of measurements with demonstrated quality
- Basic motivations of this course
- Qualimetry - as a tool for estimation of the results reliability
2. Validation of the measurement procedure
- method performance characteristics
- verification of fit-for-porpoise relevance
- EXCEL models for computing the quantities
of the characteristics
3. Uncertainty budget calculation in spectrochemical measurements
Kragten approach- constructing by EXCEL
4. Practical examples – training in EXCEL
HEADLINES three lectures + one practice
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Slide 8V. Kmetov, Alicante 2015
All here starts with the question:
What is a QUALITY ?
QUALITY –
the characteristics of a product or
service that bear on its ability to
satisfy stated or implied needs
ISO8402 1994 Quality Measurement and Quality
Assurance - Vocabilary
The ability of the qualitative (analyte identification)
and quantitative (accuracy, precision) data to satisfy
the requirements of their purpose
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Slide 9V. Kmetov, Alicante 2015
QUALIMETRY – what is it ?
- a part of the metrology science dealing with
quality estimation of the measurements and tests, including the
QUALITY OF THE INFORMATION provided from chemical analysis.
Systems for quality assurance and management
of the chemical analysis
Statistical tools for performance evaluations
andcomputing of the
estimators
This lecture will show how to create and apply algorithms supporting the process of
quality assessment.
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Slide 10V. Kmetov, Alicante 2015
“The analytical chemistry is a metrologicaldiscipline, which develops, optimizes and
applies processes of measurement, aiming to
receive reliable (bio-)chemical informationfrom global and certain kind from natural and
artificial objects or systems, for solving
analytical problems that arrived from the
informational needs”
Analytical Chemistry
II edition (2004 г.)
DEFINITION
Can we measure correctly ?
Is this the true result ?
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Slide 11V. Kmetov, Alicante 2015
Does the TRUE value
EXIST ?!Let each of you show how many
YELOW coins has got just now ?
The winner who has the maximum
score will receive
Bulgarian rose oil premium!
What is the number ?
Particularity?
CONVENTION!
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Metrology - science of measurement and its
application
NOTE Metrology includes all theoretical and practical aspects of measurement,
whatever the measurement uncertainty and field of application
VIM (2012) (2.2)
Metrological aspects are part of any measurement even the simplest one
Metrology in chemistry (MiC)is metrology applied to chemical analysis
The main goal of metrology is to prevent the problems between
people in the process of quantity characterization !!
UNCERTAINTY - a parameter associated with the result of a measurement, that characterises
the dispersion of the values that could reasonably be attributed to the measurand
Non-negative parameter characterizing the dispersion of the quantity values being
attributed to a measurand, based on the information used
International Vocabulary of Basic and General Terms in Metrology
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Slide 13V. Kmetov, Alicante 2015
TrainMiCTra in in g in Me t ro log y in Ch e m is t ry
TrainMiC is organised and conducted by
JRC-IRMM as a common international
information platform to be used as a tool for
the education in metrology in chemistry.
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Slide 14V. Kmetov, Alicante 2015
www.bipm.org/utils/.
../jcgm/JCGM_200_2012.pdf
http://www.cem.es/sites/default/files/vim-cem-2012web.pdf
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Slide 15V. Kmetov, Alicante 2015
http://www.erm-
crm.org/ERM_products/application_notes/application_note_1/D
ocuments/erm_application_note_1_spanish_rev3.pdf
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Slide 16V. Kmetov, Alicante 2015
UNCERTAINTY
Every PROCESS predetermines a PRODUCT
Every PRODUCT possess characteristics – qualities
Every quantitatively defined characteristics can be measured
the total uncertainty:
Dispersion of the product characteristics
+
Dispersion of the measurement procedure
_____________________________________________________
= total dispersion -> UNCERTAINTY
Result = Value ± Uncertainty (units)
a parameter associated with the result of a measurement, that characterises
the dispersion of the values that could reasonably be attributed to the measurand
Non-negative parameter characterizing the dispersion of the quantity values
being attributed to a measurand, based on the information used
International Vocabulary of Basic and General Terms in Metrology
there is a change in the treatment
of measurement uncertainty from
an
Error Approach (sometimes
called Traditional Approach or True
Value Approach)
to
an Uncertainty Approach
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Slide 17V. Kmetov, Alicante 2015
..from an Error Approach (Traditional or True
Value Approach) to an Uncertainty Approach..
The objective of measurement in the Error Approach
is to determine an estimate of the true value that is
as close as possible to that single true value. The
deviation from the true value is composed of random
and systematic errors.
… The objective of measurement in the Uncertainty
Approach is not to determine a true value as closely
as possible. Rather, it is assumed that the information
from measurement only permits
assignment of an interval
of reasonable values to the measurand,
based on the assumption that no mistakes have been
made in performing the measurement. Joint Committee for
Guides in Metrology
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Slide 18V. Kmetov, Alicante 2015
Do you believe,
that one table spoon of water contains
more water molecules
than spoons of water into the ocean ?
OCEAN (volume) = 𝟏. 𝟑 𝟏𝟎𝟗 𝒌𝒎𝟑 = 𝟏. 𝟑 𝟏𝟎𝟗x 𝟔. 𝟔𝟕 𝟏𝟎 𝟏𝟑 spoons = 𝟖. 𝟔𝟕 𝟏𝟎𝟐𝟐 spoons
𝑯𝟐𝑶 𝒊𝒏𝒕𝒐 𝒕𝒉𝒆 𝑶𝑪𝑬𝑨 𝑵 = 𝟗 𝟏𝟎𝟐𝟐 spoons
𝟏𝒎𝒐𝒍 𝑯𝟐𝑶 = 𝟔. 𝟎𝟐𝟐 𝟏𝟎𝟐𝟑 H−O−H = 𝟏𝟖. 𝟎𝟏𝟓𝟑 𝒈
1 spoon = 𝟏𝟓 𝒈 =𝟏𝟓
𝟏𝟖𝒈 = 𝟎. 𝟖𝟑 mol
1 table spoon = 𝟎. 𝟖𝟑 x 𝟔. 𝟎𝟐𝟐 𝟏𝟎𝟐𝟑 H−O−H = 5 𝟏𝟎𝟐𝟑 H−O−H
1 table spoon = 50 𝟏𝟎𝟐𝟐 H−O−H / 2
x 2
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Slide 20V. Kmetov, Alicante 2015
How to GUARANTEE
reliability of the measurement result
Standartirized
MethodsValidated
Methods
THE TRUST
Fully documented
measurement procedure
by a transparent, clear
and standartirized
approach
Conformation trough
examination of a given item
and provision of objective
evidence that it fulfils the
requirements for a stated
intended use (VIM 2.28)
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Slide 21V. Kmetov, Alicante 2015
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Slide 22V. Kmetov, Alicante 2015
http://www.eurachem.org/
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Slide 23V. Kmetov, Alicante 2015
ONCE MEASURED
ACCEPTED EVERYWHERE
the Mutual Recognition Arrangement
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Slide 24V. Kmetov, Alicante 2015
http://eur-lex.europa.eu/
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Slide 25V. Kmetov, Alicante 2015Regional coordiantor
42
47
52
57
62
67
72
77
82
87
92
97
102
107
112
117
122
c
nm
ol·
L-1
-50
-40
-30
-20
-10
0
10
20
30
40
50
De
via
tio
n f
rom
mid
dle
of c
ert
ifie
d r
an
ge
in
%
IMEP- 9 : Trace elements in Water
Certified range (±U =2u c): 81.0 - 85.4 nmol·L-1
Cd
Results from all laboratories.
3 'less than' values6 values below -50%
20 values above 50%
± 10%
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Slide 26V. Kmetov, Alicante 2015
the ANALYSIS IS COMPARISON
MEASURAND (C) Signal
uncertainty
St1Х1 St1 Y1
Sample Х Sаmple Y
St2Х2 St2 Y2
St3Х3 St3 Y3
Interference exists if:
)(XfY
mxSt ff
uncertainty
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Slide 27V. Kmetov, Alicante 2015
the ANALYSIS IS COMPARISON
Interference exists if:
mxSt ff
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Slide 28V. Kmetov, Alicante 2015
REGULATIONShttp://ec.europa.eu/food/food/rapidalert/docs/rasff_annual_report_2012_infogra
ph_en.pdf
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Slide 29V. Kmetov, Alicante 2015
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Slide 30V. Kmetov, Alicante 2015
Interlaboratory comperisons
PU and Komihris
ICP-OES
ICP-OES ICP-MS ppb In SOLUTION2.6 2.8 Cd Sunflower seed 1
0.89 1.0 Cd Sunflower seed 24.3 5 Cd Bread49 51 Cu Sunflower seeds 175 81.0 Cu Sunfower seeds 236 39.5 Cu Bread
174 164 Zn Sunflower seed 1245 243.0 Zn Sunflower seed 2110 115 Zn Bread
Y Rh IS
Sensitivity Drift
< 5 % < 5 %
ICP-MS
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Slide 31V. Kmetov, Alicante 2015
22
'
labPT
PTlab
SS
XXZ
PT estimation,
ІZ’І 2 excellent
2< ІZ’І 3 satisfied
ІZ’І >3 unsatisfied
ICP-MS ICP-MS
Interlaboratory comparisons
PU and Alimenti
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Slide 32V. Kmetov, Alicante 2015
ICP-MS
PT
PTlab
S
XXZ
Interlaboratory comparison
PU and Alimenti
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Slide 33V. Kmetov, Alicante 2015
The role of measurement
uncertainty in:
1. Repeatability and reproducibility limits
assessment
2. Accuracy assessment by using CRM
3. Conformity assessment
4. Maximum standard measurement
uncertainty (Uf).
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Slide 34V. Kmetov, Alicante 2015
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Slide 35V. Kmetov, Alicante 2015
rXX 21
rrrrrr SSSSSuuuU 82.2)41.1(222222 2222
2
2
1
rr uUr 2
Applying к=2 for P = 95%
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Slide 36V. Kmetov, Alicante 2015
The role of measurement
uncertainty in:
1. Repeatability and reproducibility limits
assessment
2. Accuracy assessment by using CRM
3. Conformity assessment
4. Maximum standard measurement
uncertainty (Uf).
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Slide 37V. Kmetov, Alicante 2015
Accuracy estimation
CRMmm CC 22
CRMm uuu uU 2<
To evaluate the method accuracy one could compare the difference between
the Cm measured and the certified CCRM
The obtained Δm have to be compared with the UΔ:
if Δm ≤ UΔ,
there is no significant difference between the measured result and certified value
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Slide 38V. Kmetov, Alicante 2015
ACCURACY ASSESSMENT
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Slide 39V. Kmetov, Alicante 2015
The role of measurement
uncertainty in:
1. Repeatability and reproducibility limits
assessment
2. Accuracy assessment by using CRM
3. Conformity assessment
4. Maximum standard measurement
uncertainty (Uf).
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Slide 40V. Kmetov, Alicante 2015
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Slide 41V. Kmetov, Alicante 2015
References
http://www.eurachem.org/index.php/pub
lications/guides/uncertcompliance
JCGM 106:2012 - Conformity
assessment is any activity undertaken
to determine, directly or indirectly,
whether
a product, process, system, person or
body meets relevant standards and
fulfills specified requirements.
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Slide 43V. Kmetov, Alicante 2015
Conformity assessment
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Slide 44V. Kmetov, Alicante 2015
The role of measurement
uncertainty in:
1. Repeatability and reproducibility limits
assessment
2. Accuracy assessment by using CRM
3. Conformity assessment
4. Maximum standard measurement
uncertainty (Uf).
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Slide 45V. Kmetov, Alicante 2015
2
2
)1.0(2
CLOD
U f
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Slide 46V. Kmetov, Alicante 2015
Horwitz TRUMPET
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Slide 47V. Kmetov, Alicante 2015
Regulation 333
2
2
)1.0(2
CLOD
U f
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Slide 48V. Kmetov, Alicante 2015
Maximum standard
measurement
uncertainty (Uf).
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Slide 49V. Kmetov, Alicante 2015
The analyst must know:
CHEMISTRY
Normative and regulations
StatisticsMathematical
modeling
METROLOGYInstrumental
analysis
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Slide 50V. Kmetov, Alicante 2015
QUALIMETRY – what is it ?
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Slide 51V. Kmetov, Alicante 2015
http://web.ua.es/en/actualidad-universitaria/2015/marzo2015/marzo2015-9-15/la-universidad-bulgara-de-plovdiv-utilizara-el-campus-de-la-ua-como-
modelo.html
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Slide 52V. Kmetov, Alicante 2015
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Slide 53V. Kmetov, Alicante 2015
You are
welcome in
Bulgaria !
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Slide 54V. Kmetov, Alicante 2015