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MOLS8252 – Analytical Measurement Uncertainty and Method Validation

2020 – Session 1, Weekday attendance, North Ryde

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Students should consult iLearn for revised unit information.

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General Information

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Unit convenor and teaching staff Unit convenor and teaching staff Lecturer
Danny Wong
danny.wong@mq.edu.au
Contact via (02) 9850 8300
Room 235, 4 Wally's Walk
Credit points Credit points
10
Prerequisites Prerequisites
Admission to GradDipBiotech or GradCertLabAQMgt or GradDipLabAQMgt or MBiotech or MBioBus or MLabAQMgt or MRadiopharmSc or MSc or MScInnovationChemBiomolecularSc
Corequisites Corequisites
Co-badged status Co-badged status
MOLS7252
Unit description Unit description
Chemical measurements are required in forensic science, local and international trade, manufacture and production, government regulatory agencies, biotechnology, and nearly every field of science. However, there are always uncertainties associated with measurements owing to experimental errors. This unit systematically covers the estimation principles of measurement uncertainty of values deriving from analytical chemistry measurement procedures and a logical approach to the process of validating an analytical chemistry measurement method. These will then be applied to specific examples from common analytical chemistry.

Important Academic Dates

Information about important academic dates including deadlines for withdrawing from units are available at https://www.mq.edu.au/study/calendar-of-dates

Learning Outcomes

On successful completion of this unit, you will be able to:

  • ULO1: Interpret the concept of making valid analytical measurements
  • ULO2: Identify and then evaluate analytical method performance characteristics
  • ULO4: Deconstruct an analytical method in order to identify factors that influence the final result
  • ULO3: Describe the requirements for valid measurements with respect to international standards
  • ULO5: Evaluate the validity of chemical data using commonly applied statistical techniques

Assessment Tasks

Coronavirus (COVID-19) Update

Assessment details are no longer provided here as a result of changes due to the Coronavirus (COVID-19) pandemic.

Students should consult iLearn for revised unit information.

Find out more about the Coronavirus (COVID-19) and potential impacts on staff and students

General Assessment Information

In order to complete this unit satisfactorily students must

  1. submit satisfactory efforts at 3 assignments;
  2. submit a satisfactory PowerPoint presentation file for a project;
  3. perform satisfactorily in a final examination of three hours duration.

Delivery and Resources

Coronavirus (COVID-19) Update

Any references to on-campus delivery below may no longer be relevant due to COVID-19.

Please check here for updated delivery information: https://ask.mq.edu.au/account/pub/display/unit_status

Technology Used

It is important that you have a scientific calculator as hand-held calculators will be used for assignments and in the final examination.  Note that text retrieval calculators are not allowed in the final examination.

Use will be made of Excel and other data processing and display software.  Computers carrying this software are available in the teaching laboratories.  Items of interest, links to other on-line material will be placed on the unit website.

Prescribed text

J.N.Miller, J,C.Miller, R.D.Miller, Statistics and Chemometrics for Analytical Chemistry, 7th Edition, Pearson Prentice Hall, 2018 (ISBN: 978-1-292-18671-9)

Recommended references 

D.C.Montgomery, Design and Analysis of Experiments, 6th Edition, John Wiley & Sons, 2005 (ISBN: 0 471 48735 X)

R.G.Brereton, Applied Chemometrics for Scientists, John Wiley & Sons, 2007 (ISBN: 978 0 470 01686 2)

J.Lawson, J.Erjavec, Modern Statistics for Engineering and Quality Improvement, Duxbury Thomson Learning, 2001 (ISBN: 0 534 19050 2)

Eurachem/CITAC Guide: Traceability in Chemical Measurement, Eurachem and CITAC, 2003

ISO/IEC International Standard 17025 General Requirements for the competence of testing and calibration laboratories, ISO, 2005

In House Method Validation: A guide for Chemical Laboratories, LGC Ltd, 2003

Eurachem Guide: the Fitness for purpose of analytical methods, LGC Ltd, 1988

Eurachem/CITAC Guide CG4: Quantifying Uncertainty in Analytical Measurement 2nd Edition, Eurachem & CITAC, 2000

L.Kirkup, Data Analysis with Excel: An introduction for physical scientists, Cambridge University Press, 2002

D.B.Hibbert, Quality Assurance for the Analytical Chemistry Laboratory, Oxford University Press, 2007

Useful websites

Eurachem -http://www.eurachem.org/

NIST/SEMATECH Engineering Statistics Handbook http://www.itl.nist.gov/div898/handbook/index.htm

Valid Analytical Measurements http://www.vam.org.uk/home.asp

CITAC - http://www.citac.cc/

AOAC - http://www.aoac.org/

NATA - http://www.nata.com.au/publication-updates and download “Technical Note 17”.

Unit Schedule

Coronavirus (COVID-19) Update

The unit schedule/topics and any references to on-campus delivery below may no longer be relevant due to COVID-19. Please consult iLearn for latest details, and check here for updated delivery information: https://ask.mq.edu.au/account/pub/display/unit_status

Proposed schedule

 

Week 1 + 2
  • Statistics
  • Samples and populations
  • Standard deviation of the mean
  • Trueness and precision
  • Significance testing
    • t-test for two means
    • F-test for two variances
    • Grubb’s test for outliers
    • c2 test
  • Confidence intervals
  • Degrees of freedom
  • Calibration and regression
    • The correlation coefficient
    • Standard error of the slope
    • Standard error of the intercept
    • Standard error of prediction
  • Basic ANOVA, Two-way ANOVA

 

 

Week 3
  • Non-linear calibration
    • Procedure
    • Standard error of prediction
  • What is validation?
  • What is measurement uncertainty?
  • The importance of analytical measurements
  • What makes a method valid?
  • Fitness for purpose
  • Statistical control (control /Shewhart / CuSum charts)

 

 

Week 4
  • Review of documents related to validation
    • ISO 17025
    • IUPAC technical report 2002
    • ICH guidelines 2005
    • Joint AOAC/FAO/IAEA/IUPAC food standard programme
  • ISO 17025 and validation
  • ISO 17025 and NATA
  • IUPAC technical report and validation
  • AOAC / FAO / IAEA / IUPAC and validation
  • ICH guidelines on validation
  • Other documents on validation
  • Verification

 

 

Week 5
  • Method validation as part of method development
  • Determination of performance characteristics
  • Key performance characteristics
    • Confirmation of identity
    • Selectivity
    • Limit of detection
    • Limit of quantification
    • Working and linear range
    • Sensitivity
    • Accuracy
    • Precision – Repeatability and Reproducibility
    • Recovery

 

 

Week 6 + 8
  • Further validation
    • Equipment calibration
    • Quality control checks, Shewhart control chart
    • Ruggedness and Robustness
  • Ruggedness testing and experiment designs
  • Factorial designs
    • 22 factorial designs
    • 23 factorial designs

 
  • Optimisation experiments
  • Response surface concepts and methods
  • Central composite designs
  • Box-Behnken designs
  • Graphical interpretation of response surfaces
  • Simplex designs

 
  •  

Week 9
  • Measurement uncertainty
  • Why is measurement uncertainty important?
  • The ISO GUM
  • The uncertainty estimation process
  • Specification of a measurand
  • Sources of uncertainties
  • Types of uncertainties

Cause and effect diagram for use in measurement uncertainty estimation

 

 

Week 10
  • Quantifying uncertainties
  • Converting uncertainties to standard uncertainties
  • Combining uncertainties
    • Mathematical expression for the propagation of uncertainties
    • Rules for combining uncertainties
    • Sensitivity coefficients

 

 
     

 

 

Week 11
  • Expanded uncertainties
  • Coverage factors
  • Degrees of freedom
  • The Welch-Satterthwaite equation
    • Reporting results
    • Client education
    • Tools for uncertainty education – The spreadsheet method of measurement uncertainty estimation
  • Measurement uncertainty from a calibration plot

 

 

Week 12
  • Traceability
  • Why is it important?
  • Stated references: SI units
  • Traceability and uncertainty

Measurement uncertainty - a worked example from start to finish

 

 

Week 13
  • Bias and measurement uncertainty
  • Other approaches to measurement uncertainty
  • Bottom up methods
  • Top down methods
  • Inter-laboratory studies
  • Verification of standard methods

 

 

 

 

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