Laboratory Quality Control
Code
11266
Academic unit
Faculdade de Ciências e Tecnologia
Department
Departamento de Química
Credits
3.0
Teacher in charge
Marco Diogo Richter Gomes da Silva
Weekly hours
2
Total hours
28
Teaching language
Português
Objectives
This course will include fundamental aspects of results quality control in laboratory. It is intended to apply metrology methods to the analysis of quality parameters (examples: calculate calibration uncertainties, defining criteria for acceptance of certificates of calibration). Further includes the representation of the sampling, sampling methods for chromatography and result treatments and the comparison and calibration and associated statistical principles.
Prerequisites
Analytical chemistry
Subject matter
1. Objectives of Physical-chemical validation methods: What methods to validate. Objectives of Physical-chemical quality control tests.
2. Management and laboratory infrastructure, materials, equipment, instruments and other devices; Working Procedures
3. Methods for chromatography sample preparation. Brief review of methods for sample preparation. Liquid-liquid extraction: distribution coefficient, distribution ratio, simple extraction and multiple extractions. Micro liquid-liquid extraction (LLME) dispersive liquid-liquid microextraction (DLLME), solid phase extraction (SPE), solid phase microextraction (SPME) procedures (direct and headspace); desorption / deabsorption in gas and liquid chromatography; kinetic aspects; quantification; fiber coatings; practical aspects to consider (coating thickness, pH, temperature, agitation, fiber position, derivatization, effect of salts). Examples of applications. dispersion of the solid phase matrix (MSPD - Quenchers): principles and applications, supercritical fluid extraction. Brief notions in sampling.
4. Brief Statistical notions applied in validation methods: Normal Distribution, Confidence Intervals, Descriptive Statistics, location parameters and dispersion, statistical inference, hypothesis testing: F test and t-test.
5. Validation parameters. Performance characteristics of the methods: Selectivity, working range, linearity, sensitivity, limits of detection and quantification, precision (repeatability, intra-and interlaboratory reproducibility), trueness (bias), Robustness
6. Internal quality control tests: Analysis of blanks, replicate analyzes, analysis of spiked samples, analysis of internal reference materials, quality control limits of detection and / or quantification, Sensitivity Control, Control and Acceptance Charts
7. Physico-chemical External quality tests: Participation in fitness tests, Analysis of Certified Reference Materials
8. Comparison of more than two sets of results
Bibliography
1. Practical Statistics for the Analytical Scientist. A Bench Guide, 2nd Edition, Stephen L R Ellison, Vicki J Barwick, Trevor J Duguid Farrant, The Royal Society of Chemistry, Cambridge CB4 0WF, UK
2. Statistics and Chemometrics for Analytical Chemistry, Fifth Edition, James N. Miller, Jane C. MillerPearson Education Limited, Essex CM20 2JE, England
3. Guides and relevant documentation in the field of validation of Physical-Chemical methods
Teaching method
Theorical courses and seminars. Reports in group.
Evaluation method
SEMINAR LIKE UC
The evaluation is based on groupwork of 3 or 4 persons
1 poster presentation in A3 or A4 format - P
1 oral presentation of 15 minutes with 5 minutes discussion - AO
1 "Note", short comunication - N
All entries must be written in English, with the presentation of AO performed in Portuguese or English
The final grade is a weighted average of all of the above components:
Final Grade = (P + TO + N) / 3
According to the evaluation rules the seminar/continued evaluation grades can not be improved in the same scholar year