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ESTIMATION OF MEASUREMENT
UNCERTAINTY:
A REQUIREMENT FOR ISO 17025
ACCREDITATION
Dotun Bolade
Managing Consultant
Dotun Bolade is an Analytical Chemist/Environmental Scientist by training
and practice has spent the past five years working in Nigeria’s Oil and Gas
industry. For him, ISO management systems have become second nature
having worked in environments where ISO 9001, 14001, 18001 and 17025
have been fully implemented/accredited. He is a Certified PECB ISO/IEC
17025 Lead Assessor, ISO 14001, 9001 & 29001 Lead Implementer and
Certified Trainer. Dotun is a PECB Partner and Managing Consultant,
EN2SOL PNP LIMITED.
Contact Information
2348066884793
Dotun.bolade@energysolutiosng.com
www.domain.com
linkedin.com/Dotun Bolade
twitter.com/dotunBolade
Objectives:
 To introduce the basic concepts related to measurement
results and measurement uncertainty & their relevance to
chemical data
 Introduce mathematical concepts, uncertainty sources and
important approaches for estimation of measurement
uncertainty
 Understand availability and relevance of data in estimating
measurement uncertainty
 Understand selection of suitable approach for uncertainty
measurement based on available data
Content:
 Introduction
 Accuracy, Precision &
Trueness
 Sources of Uncertainty
in Measurement
 Concepts in
Uncertainty estimation
 Elements of an
Uncertainty Budget
 Uncertainty
Calculation in
Pipetting; an
example
 References
Introduction:
Key Terms:
 Measurement/Chemical Analysis
 Uncertainty/Uncertainty Range
 Measurand
 True Value
 Measured Value
 Error (systematic & random)
Accuracy, Precision & Trueness:
Common Sources of Uncertainty in
Measurement:
 Equipment
 Unit Under Test
 Operator
 Method
 Calibration
 Environment
Uncertainty in
Volumetric
Measurements:
o Repeatability Uncertainty
o Calibration Uncertainty
o Temperature Uncertainty
o Application-Specific
Uncertainty
Concepts in Uncertainty Estimation:
 Normal Distribution
Concepts in Uncertainty Estimation:
 T-Distribution
Elements of an Uncertainty Budget:
 Repeatability
 Reproducibility
 Stability
 Bias
 Drift
 Resolution
 Reference Standard
 Reference Standard
Stability
To calculate Repeatability:
 Repeat a measurement
‘n’ number of times
 Record the results of
each measurement.
 Calculate the standard
deviation.
Reproducibility:
Common comparisons for Reproducibility Testing:
Operator vs Operator Reproducibility
Equipment vs Equipment Reproducibility
Method vs Method Reproducibility
Day vs Day Reproducibility
Environment vs Environment Reproducibility
To calculate Reproducibility:
 Perform a Repeatability Test
 Calculate the mean of average
 Change a variable and repeat the Repeatability Test
 Calculate the mean or average.
 Calculate the standard deviation of the test averages
Stability:
Property of a measuring instrument,
whereby its metrological properties
remain constant in time
To calculate Stability:
 Review your last 3 calibration reports
 Record the results from each calibration report
 Calculate the standard deviation of the
calibration results.
Bias:
 Estimate of systematic measurement error
 Average of replicate indication minus a
reference quantity value
To calculate Bias:
 Review your latest calibration report
 Find the As Left value or measurement result
 Find the Nominal value or standard value
 Calculate the difference.
Drift:
 Continuous or incremental change over time
in indication, due to changes in metrological
properties of a measuring instrument
To calculate Drift:
 Review your last 3 calibration reports
 Record the results from each calibration report
 Record the date each calibration was performed
 Calculate the average daily drift rate
 Multiply the average daily drift rate by your
calibration interval (in days).
Resolution:
 Smallest change in a quantity being
measured that causes a perceptible change
in the corresponding indication
To Find Resolution:
 Look at your measurement system or
equipment
 Find the least significant digit
 Observe the smallest incremental change
Reference Standard Uncertainty:
 Uncertainty of a measurement standard designated for
the calibration of other measurement standards for
quantities of a given kind in a given organization or at a
given location
 Reference standard uncertainty should be included in
the every uncertainty budget.
To Calculate Reference Standard Uncertainty:
 Review your latest calibration report
 Find the reported estimate of measurement
uncertainty
Reference Standard Stability:
 stability of a measurement standard designated for the
calibration of other measurement standards for
quantities of a given kind in a given organization or at a
given location
 Reference standard uncertainty should be included in
the every uncertainty budget.
To Calculate Reference Standard Stability:
 Review your last 3 calibration reports
 Record the uncertainty estimate from each calibration report
 Calculate the standard deviation.
Uncertainty Calculation in Pipetting:
Uncertainty Calculation in Pipetting:
In calculating the volume and Uncertainty of
liquid delivered from a self-calibrated volumetric
pipette, there are 3 main uncertainty
components;
Uncertainty due to repeatability, u(V,rep)
Uncertainty due to pipette calibration, u(V,cal)
Uncertainty due to the temperature difference
from 20 °C, u(V,temp).
Uncertainty Calculation in Pipetting:
In calculating the volume and Uncertainty of
liquid delivered from a self-calibrated volumetric
pipette, there are 3 main uncertainty
components;
Uncertainty due to repeatability, u(V,rep)
Uncertainty due to pipette calibration, u(V,cal)
Uncertainty due to the temperature difference
from 20 °C, u(V,temp).
Uncertainty Calculation in Pipetting:
Uncertainty due to
repeatability of
pipetting u (V, REP)
is equal to this
standard deviation
0.0057 ml
Uncertainty Calculation in Pipetting:
Uncertainty of the calibration is
expressed (when calibration is done)
as the standard deviation of the mean:
Uncertainty Calculation in Pipetting:
When there is a possibility that pipetting is
performed at a different temperature from
the calibration (and this possibility exists
almost always), then an additional
uncertainty source due to temperature
change is introduced and it has to be taken
into account.
Uncertainty Calculation in Pipetting:
Combined Standard Uncertainty:
When estimating the standard uncertainty of an
output quantity then the standard uncertainties of all
input quantities are taken into account
The standard uncertainty of the output quantity
obtained in this way is called combined standard
uncertainty
Uncertainty Calculation in Pipetting:
Expanded Uncertainty:
• Expanded uncertainty is calculated from the
standard uncertainty by multiplying it with
a coverage factor, k.
• In the case of the pipetting example the k = 2
expanded uncertainty is found as follows:
U(V ) = uc(V ) · k = 0.0077 · 2 = 0.0154 ml
Uncertainty Calculation in Pipetting:
Summary:
The volume of the pipetted liquid is:
V = (9.992 ± 0.015) ml, k = 2, norm
The parentheses (brackets) mean that the unit “ml” is valid
both for the value and the uncertainty. “norm.” means that
the output quantity is expected to be approximately
normally distributed. This, together with coverage factor
value 2, means that the presented uncertainty is expected to
corresponds to approximately 95% coverage probability
References:
• A2LA. (2015). R205 – Specific Requirements: Calibration
Laboratory Accreditation Program. Frederick: A2LA.
• JCGM. (2012). International Vocabulary of Metrology:
Basic and General Concepts and Associated Terms. Sèvres:
BIPM.
• Estimation of Measurement Uncertainty in Chemical
Analysis. Available at https://sisu.ut.ee/measurement/10-
approach-based-validation-and-quality-control-data-top-
down-approach
ISO 17025 Training Courses
 ISO/IEC 17025 Introduction
1 Day Course
 ISO/IEC 17025 Foundation
2 Days Course
 ISO/IEC 17025 Lead Implementer
5 Days Course
 ISO/IEC 17025 Lead Assessor
5 Days Course
Exam and certification fees are included in the training price.
https://pecb.com/iso-iec-17025-lead-assessor | www.pecb.com/events
THANK YOU
?
2348066884793
dotun.bolade@energysolutionsng.com
linkedin.com/Dotun Bolade
twitter.com/dotunBolade
oladotunbolade@gmail.com

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Estimation of Measurement Uncertainty

  • 1. ESTIMATION OF MEASUREMENT UNCERTAINTY: A REQUIREMENT FOR ISO 17025 ACCREDITATION
  • 2. Dotun Bolade Managing Consultant Dotun Bolade is an Analytical Chemist/Environmental Scientist by training and practice has spent the past five years working in Nigeria’s Oil and Gas industry. For him, ISO management systems have become second nature having worked in environments where ISO 9001, 14001, 18001 and 17025 have been fully implemented/accredited. He is a Certified PECB ISO/IEC 17025 Lead Assessor, ISO 14001, 9001 & 29001 Lead Implementer and Certified Trainer. Dotun is a PECB Partner and Managing Consultant, EN2SOL PNP LIMITED. Contact Information 2348066884793 Dotun.bolade@energysolutiosng.com www.domain.com linkedin.com/Dotun Bolade twitter.com/dotunBolade
  • 3. Objectives:  To introduce the basic concepts related to measurement results and measurement uncertainty & their relevance to chemical data  Introduce mathematical concepts, uncertainty sources and important approaches for estimation of measurement uncertainty  Understand availability and relevance of data in estimating measurement uncertainty  Understand selection of suitable approach for uncertainty measurement based on available data
  • 4. Content:  Introduction  Accuracy, Precision & Trueness  Sources of Uncertainty in Measurement  Concepts in Uncertainty estimation  Elements of an Uncertainty Budget  Uncertainty Calculation in Pipetting; an example  References
  • 5. Introduction: Key Terms:  Measurement/Chemical Analysis  Uncertainty/Uncertainty Range  Measurand  True Value  Measured Value  Error (systematic & random)
  • 7. Common Sources of Uncertainty in Measurement:  Equipment  Unit Under Test  Operator  Method  Calibration  Environment Uncertainty in Volumetric Measurements: o Repeatability Uncertainty o Calibration Uncertainty o Temperature Uncertainty o Application-Specific Uncertainty
  • 8. Concepts in Uncertainty Estimation:  Normal Distribution
  • 9. Concepts in Uncertainty Estimation:  T-Distribution
  • 10. Elements of an Uncertainty Budget:  Repeatability  Reproducibility  Stability  Bias  Drift  Resolution  Reference Standard  Reference Standard Stability To calculate Repeatability:  Repeat a measurement ‘n’ number of times  Record the results of each measurement.  Calculate the standard deviation.
  • 11. Reproducibility: Common comparisons for Reproducibility Testing: Operator vs Operator Reproducibility Equipment vs Equipment Reproducibility Method vs Method Reproducibility Day vs Day Reproducibility Environment vs Environment Reproducibility To calculate Reproducibility:  Perform a Repeatability Test  Calculate the mean of average  Change a variable and repeat the Repeatability Test  Calculate the mean or average.  Calculate the standard deviation of the test averages
  • 12. Stability: Property of a measuring instrument, whereby its metrological properties remain constant in time To calculate Stability:  Review your last 3 calibration reports  Record the results from each calibration report  Calculate the standard deviation of the calibration results.
  • 13. Bias:  Estimate of systematic measurement error  Average of replicate indication minus a reference quantity value To calculate Bias:  Review your latest calibration report  Find the As Left value or measurement result  Find the Nominal value or standard value  Calculate the difference.
  • 14. Drift:  Continuous or incremental change over time in indication, due to changes in metrological properties of a measuring instrument To calculate Drift:  Review your last 3 calibration reports  Record the results from each calibration report  Record the date each calibration was performed  Calculate the average daily drift rate  Multiply the average daily drift rate by your calibration interval (in days).
  • 15. Resolution:  Smallest change in a quantity being measured that causes a perceptible change in the corresponding indication To Find Resolution:  Look at your measurement system or equipment  Find the least significant digit  Observe the smallest incremental change
  • 16. Reference Standard Uncertainty:  Uncertainty of a measurement standard designated for the calibration of other measurement standards for quantities of a given kind in a given organization or at a given location  Reference standard uncertainty should be included in the every uncertainty budget. To Calculate Reference Standard Uncertainty:  Review your latest calibration report  Find the reported estimate of measurement uncertainty
  • 17. Reference Standard Stability:  stability of a measurement standard designated for the calibration of other measurement standards for quantities of a given kind in a given organization or at a given location  Reference standard uncertainty should be included in the every uncertainty budget. To Calculate Reference Standard Stability:  Review your last 3 calibration reports  Record the uncertainty estimate from each calibration report  Calculate the standard deviation.
  • 19. Uncertainty Calculation in Pipetting: In calculating the volume and Uncertainty of liquid delivered from a self-calibrated volumetric pipette, there are 3 main uncertainty components; Uncertainty due to repeatability, u(V,rep) Uncertainty due to pipette calibration, u(V,cal) Uncertainty due to the temperature difference from 20 °C, u(V,temp).
  • 20. Uncertainty Calculation in Pipetting: In calculating the volume and Uncertainty of liquid delivered from a self-calibrated volumetric pipette, there are 3 main uncertainty components; Uncertainty due to repeatability, u(V,rep) Uncertainty due to pipette calibration, u(V,cal) Uncertainty due to the temperature difference from 20 °C, u(V,temp).
  • 21. Uncertainty Calculation in Pipetting: Uncertainty due to repeatability of pipetting u (V, REP) is equal to this standard deviation 0.0057 ml
  • 22. Uncertainty Calculation in Pipetting: Uncertainty of the calibration is expressed (when calibration is done) as the standard deviation of the mean:
  • 23. Uncertainty Calculation in Pipetting: When there is a possibility that pipetting is performed at a different temperature from the calibration (and this possibility exists almost always), then an additional uncertainty source due to temperature change is introduced and it has to be taken into account.
  • 24. Uncertainty Calculation in Pipetting: Combined Standard Uncertainty: When estimating the standard uncertainty of an output quantity then the standard uncertainties of all input quantities are taken into account The standard uncertainty of the output quantity obtained in this way is called combined standard uncertainty
  • 25. Uncertainty Calculation in Pipetting: Expanded Uncertainty: • Expanded uncertainty is calculated from the standard uncertainty by multiplying it with a coverage factor, k. • In the case of the pipetting example the k = 2 expanded uncertainty is found as follows: U(V ) = uc(V ) · k = 0.0077 · 2 = 0.0154 ml
  • 26. Uncertainty Calculation in Pipetting: Summary: The volume of the pipetted liquid is: V = (9.992 ± 0.015) ml, k = 2, norm The parentheses (brackets) mean that the unit “ml” is valid both for the value and the uncertainty. “norm.” means that the output quantity is expected to be approximately normally distributed. This, together with coverage factor value 2, means that the presented uncertainty is expected to corresponds to approximately 95% coverage probability
  • 27. References: • A2LA. (2015). R205 – Specific Requirements: Calibration Laboratory Accreditation Program. Frederick: A2LA. • JCGM. (2012). International Vocabulary of Metrology: Basic and General Concepts and Associated Terms. Sèvres: BIPM. • Estimation of Measurement Uncertainty in Chemical Analysis. Available at https://sisu.ut.ee/measurement/10- approach-based-validation-and-quality-control-data-top- down-approach
  • 28. ISO 17025 Training Courses  ISO/IEC 17025 Introduction 1 Day Course  ISO/IEC 17025 Foundation 2 Days Course  ISO/IEC 17025 Lead Implementer 5 Days Course  ISO/IEC 17025 Lead Assessor 5 Days Course Exam and certification fees are included in the training price. https://pecb.com/iso-iec-17025-lead-assessor | www.pecb.com/events