Unit convenor and teaching staff |
Unit convenor and teaching staff
Unit Convenor
Danny Wong
Contact via danny.wong@mq.edu.au
F7B 235
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Credit points |
Credit points
4
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Prerequisites |
Prerequisites
Admission to MLabQAMgt or PGDipLabQAMgt or PGCertLabQAMgt or MSc
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Corequisites |
Corequisites
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Co-badged status |
Co-badged status
CBMS860 is co-badged with CBMS760.
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Unit description |
Unit description
This unit covers the estimation principles of measurement uncertainty of values deriving from analytical chemistry measurement procedures and a systematic approach to the process of validating an analytical chemistry measurement method. These will then be applied to specific examples from common analytical chemistry.
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Information about important academic dates including deadlines for withdrawing from units are available at https://www.mq.edu.au/study/calendar-of-dates
On successful completion of this unit, you will be able to:
Name | Weighting | Due |
---|---|---|
Assignments | 30% | To be decided |
Project | 15% | To be decided |
Mid-Year 3-hour Examination | 55% | June 2014 |
Due: To be decided
Weighting: 30%
Due: To be decided
Weighting: 15%
Due: June 2014
Weighting: 55%
· Timetable: Please check http://www.timetables.mq.edu.au/for the official timetable of the unit.
· Lectures:Thematerialpresentedinthelecturesisimportantandyoushouldnotassumethatall examinable material is available in the textbook or in printed notes. On the other hand, do not assume that all examinable material is to be found in the lecture notes.
· Tutorial: A weekly one-hour tutorial session will immediately follow the lectures. ·Laboratory Work: There is no laboratory work in this unit.
Lecture materials are located in the website for CBMS860 at at https://ilearn.mq.edu.au.
Macquarie University provides a range of Academic Student Support Services. Details of these services can be accessed at http://www.students.mq.edu.au.
Week 1 + 2•Statistics
•Samples and populations
•Standard deviation of the mean
•Trueness and precision
•Significance testing
ot-test for two means
oF-test for two variances
oGrubb’s test for outliers
oχ2 test
•Confidence intervals
•Degrees of freedom
•Calibration and regression
oThe correlation coefficient
oStandard error of the slope
oStandard error of the intercept
oStandard error of prediction
•Basic ANOVA, Two-way ANOVA
Week 3•Non-linear calibration
oProcedure
oStandard 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
Week 4•Review of documents related to validation
oISO 17025
oIUPAC technical report 2002
oICH guidelines 2005
oJoint 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
oConfirmation of identity
oSelectivity
oLimit of detection
oLimit of quantification
oWorking and linear range
oSensitivity
oAccuracy
oPrecision – Repeatability and Reproducibility
oRecovery
Week 6•Further validation
oEquipment calibration
oQuality control checks, Shewhart control chart
oRuggedness and Robustness
•Ruggedness testing and experiment designs
•Factorial designs
o22 factorial designs
o23 factorial designs
oFractional factorial designs
oThe Plackett-Burman designs
Week 7•Optimisation experiments
oResponse surface concepts and methods
oCentral composite designs
oGraphical interpretation of response surfaces
oSimplex designs
Week 8•Multivariate data analysis
oPrincipal components analysis
oBackground
oScores and loadings
oAlgorithm
oGraphical representation
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
oMathematical expression for the propagation of uncertainties
oRules for combining uncertainties
•Sensitivity coefficients
Week 11•Expanded uncertainties
•Coverage factors
•Degrees of freedom
oThe 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
oWhy is it important?
oStated 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
oBottom up methods
oTop down methods
•Inter-laboratory studies
•Verification of standard methods
Prescribed text: J.N.Miller, J,C.Miller, Statistics and Chemometrics for Analytical Chemistry, 5th Edition, Pearson Prentice Hall, 2005 (ISBN: 0 131 29192 0) Recommended references (all available in University Library) 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/Macquarie University policies and procedures are accessible from Policy Central. Students should be aware of the following policies in particular with regard to Learning and Teaching:
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It is important that you have a scientific calculator as hand-held calculators will be used during laboratory sessions, 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 unitwebsite.
Computers for general use are provided by the University, but it would be advantageous to have your own computer and internet access.