ANALYTICAL CHEMISTRY OF PROCESS
Learning outcomes of the course unit
At the end of the course, the student should have acquired knowledge about the principles and applications of the Process Analytical Chemistry, which is exploited in industry.
In particular, the student should be able to:
- know and describe the main techniques and strategies for real-time analysis used to control an industrial process, with the final purpose of quality assurance, taking into account also security and profit aspects.
- explain how process analytical chemistry fits into a multidisciplinary approach, which also involves the use of chemiometric techniques for data elaboration and predictive statistical model building.
- connect each other the different topics addressed during the course and connect them with the basic and related disciplines; discuss critically the concepts and consult relevant scientific literature.
- apply the acquired knowledge to identify the proper analytical approaches for real-time monitoring of a chemical reaction and of an industrial process, combined to chemometric techniques for data elaboration.
- program the experimental activity for predictive models building and collect analytical information for process control.
- Evaluate critically the own knowledges and capacities, and interpret the results.
- adapt yourself to different working areas and topics and make judgments on important scientific issues.
- support the own activity on the basis of an autonomous judgment on issues pertinent to the course of study.
- interact with other people and work in a group in multidisciplinary projects, taking into account the objectives and the methods to achieve them.
- easily retrieve information from scientific literature, databases and internet.
- possess personal skills of logical reasoning and autonomous learning, to independently propose solutions for new scientific topics and professional issues related to the attended studies.
- analyse critically the results from experimental processes, by extrapolating the information necessary for process optimization.
For the course, it will be fundamental the knowledge of instrumental analytical chemistry and of basic concepts in univariate chemometrics.
Course contents summary
- Role of the analytical chemist for the monitoring and real-time analysis of industrial processes with the final aim of product quality assurance
- Sampling from process lines and sample conditioning
- Main chemometric multivariate techniques for data elaboration, result interpretation and building of predictive models
- Main types of process analyzers and their interface to chemical processes
- Examples from current literature and discussion of scientific articles
- Seminars of invited speakers from industry
- Possibly a visit to a company
Aim of process analytical chemistry. Differences between laboratory analysis and process analysis. Different requisites of process analyzers respect to lab instruments. Modalities of process analysis interface (off-line, at-line, on-line and in-line).
Concept of quality, quality by design (QbD) and process analytical technology (PAT).
Sampling from production lines and reactors, sample representativeness. Sampling frequency. Use of sampling probe and fast loops. Sample conditioning and transport.
Multivariate chemometric techniques. Basic concepts of supervised and unsupervised pattern recognition techniques: principal component analysis, cluster analysis, linear discriminant analysis, multiple linear regression, principal component regression, partial least square regression. Direct and inverse calibration. Concepts of model fitting, prevision and cross-validation. Proper choice of the calibration set for model building.
Spectroscopic techniques for process analyisis, with particular focus to vibrational spectroscopy: middle-IR, near-IR and Raman. Potentialities and limits for real-time and remote (use of optic fibers) analysis. Transmission, reflection, trasflectance, ATR (middle-IR) acquisition modes. Probe for on-line and in-line analysis. Elaboration techniques for spectra pre-treatment.
Brief mention to hyperspectral imaging for chemical imaging.
Particle size analysis. Particle size distribution, weighting concept (number-weighted, volume-weighted, .). Turbidity measurements, FBRM and particle viewers. Crystallization process monitoring.
Artificial sensing systems: electronic nose and tongue. Basic concepts, potentialities. Types of detectors.
Ion mobility spectrometry for process analytical chemistry
Discussion of literature examples.
Seminars by industrial experts speakers.
Possible visit to a company
Books (all available the Chemistry building library):
“Process Analytical Technology: Spectroscopic Tools and Implementation Strategies for the Chemical and Pharmaceutical Industries”, Edited by Katherine A. Bakeev, 2nd Edition, 2010.
“Process Analytical Chemistry. Control, Optimization, Quality, Economy”, by Karl Heinz Koch, Springer Ed., 1999.
“Process Analytical Chemistry”, Edited by F. McLennan and B.R. Kowalsky, 1st Edition, 1995.
Scientific articles, slides from seminars (at invited speaker discretion) and other material necessary for the preparation of the exam, or useful for any further supplementary study, are uploaded to the Elly platform, or otherwise expressly indicated in slides available on Elly.
Teaching activities will involve frontal lessons; if COVID-19 emergency will persist, also remote modality will be involved.
Lessons will be supported by concrete examples and study of significant cases, concerning the application of the analytical process chemistry, taken from the most recent scientific literature. In addition, in order to highlight the impact of the discussed analytical techniques and approaches in the most important industrial sectors, seminars by external experts in the field, and possibly a visit to a company active in the process analytical chemistry, will be organized.
The slides used as lesson support will be available for download on the Elly platform, where are regularly uploaded.
Slides are an integral part of the didactic material. It is important to remind that non-attending students have to check the available teaching material and the directions provided by the teacher through the Elly platform.
Assessment methods and criteria
The assessment of the student learning will be carried out through a final oral examination in presence; if due to the persistence of the COVID-19 health emergency it is necessary to integrate examination session with remote modality, remote oral exam will be performed via Teams.
During the oral exam (of about 40 min) the student must demonstrate understanding of the fundamental concepts of each topic, he/she has to be able to discuss in a critical and applicative point of view the issues dealt with and to possess a proper competence in the scientific language; the vote will be immediately communicated at the end of the exam and the student’s signature will be required for vote acceptance.