Laboratory Quality Control
Code
11266
Academic unit
Faculdade de Ciências e Tecnologia
Department
Departamento de Química
Credits
3.0
Teacher in charge
Elvira Maria Sardão Monteiro Gaspar
Weekly hours
2
Total hours
28
Teaching language
Português
Objectives
The course will include fundamental aspects of good practices in laboratory, the laboratory organization and procedures. It will include legislation (ISO 17025 and ISO 9001). The quality parameters, sampling and sample management will be also focused. Calibration procedures, method validation, Certified Reference Materials, validation of resultsand and the equirements for analytical quality as well as the process of lab quality audit will be taught.
Prerequisites
Basic knowledge in 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
Statistics and Chemometrics for Analytical Chemistry, Fifth Edition, James N. Miller, Jane C. MillerPearson Education Limited, Essex CM20 2JE, England
Pedagogic material will be given to the students during the course.
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