Learning objectives
The course aims to provide students with advanced knowledge of the analytical process, of the classification of analytical methods and of the main instrumental analytical techniques, with particular regard to spectroscopy, chromatography, mass spectrometry and electron microscopy analytical techniques: for this purpose the principles, performance and fields of applicability of the techniques are discussed with reference to the characteristics of the materials.
The aim of the course is to guide students in the choice of an analytical technique in relation to the purpose of the analysis and in addition to guide students in a critical evaluation of the experimental results in relation to the performance of the instrumental techniques, the field of investigation (qualitative analysis, quantitative or confirmatory method) and the quality parameters of the analytical methods. To this end, the concept of validation ("fitness for purpose") of analytical methods is defined and the European guidelines for validation are illustrated.
Prerequisites
Physics II and laboratory
Organic chemistry for material science
Analytical chemistry of materials
Course unit content
Introduction to instrumental analytical techniques.
Introduction to instrumental methods of analysis: quality parameters and validation. Quality of analytical data and measurement uncertainty.
Analytical methods for the characterization of materials and polymers based on chromatographic techniques. Liquid chromatography (LC): instrumentation and separation mechanisms. Size exclusion liquid chromatography (SEC) and gel permeation chromatography (GPC) for the characterization of the molecular weight distribution of polymers. Instrumentation for SEC/GPC and detection systems.
Analytical methods for the characterization of materials based on mass spectrometry. Principles of mass spectrometry (MS) and instrumentation: sample introduction system, ionization sources, analyzers, detectors, system for data acquisition and processing. Sample introduction system: gas chromatograph, liquid chromatograph. Gas chromatography (GC): outline on instrumentation and gas liquid chromatography separation mechanism. "Hard" ionization sources (EI, CI). “Soft” ionization sources (APCI, ESI, MALDI), mass analyzers and their characteristics (resolution, mass accuracy). Low-resolution mass spectrometry. High-resolution mass spectrometry. Outline on tandem mass spectrometry. Interpretation of mass spectra. Hyphenated techniques: GC-MS, LC-MS, LC-MS/MS.
Analytical methods for the characterization of inorganic materials based on atomic spectroscopy. Inductively Coupled Plasma Source Optical Emission Spectroscopy (ICP-AES). Overview of mass spectrometry with inductively coupled plasma source (ICP-MS).
Sample pre-treatment for use with atomic spectroscopy techniques. Applications of atomic spectroscopy to trace analysis of Pd, Pt and Rh in spent automobile catalysts, determination of heavy metals in virgin and used lubricating oils, trace metals testing for food contact materials.
Analytical methods for the morphological characterization and compositional analysis of materials based on electron microscopy techniques. Electron microscopy for the analysis of conductive materials (SEM). Electron microscopy for the analysis of non-conductive materials (environmental scanning electron microscopy, ESEM); energy dispersed X-ray emission (EDX) spectroscopy and element mapping (ESEM-EDX).
Laboratory activities related to applications of atomic spectroscopy, liquid chromatography, mass spectrometry and electron microscopy for the characterization of materials.
Full programme
Instrumental analytical techniques and their classification on the basis of the general principles on which they are based. Performance of analytical techniques.
Introduction to the methods of instrumental analysis. Steps of an analytical process in the development of a method. Performance of a method: choice of an analytical method depending on the materials being analyzed and the objectives of the analysis.
Classification of methods: qualitative analysis, quantitative analysis and confirmation.
The concept of "fitness for purpose" of an analytical method: validation and quality parameters of a method. Calibration of a quantitative analysis method. Quality of analytical data and measurement uncertainty.
Analytical methods for the dimensional characterization of materials and polymers based on chromatographic techniques.
Liquid chromatography (LC): notes on instrumentation and separation mechanisms. Size exclusion liquid chromatography (SEC) and gel permeation chromatography (GPC). Calibration of the GPC system for the dimensional characterization of materials: applications on polymers.
Instrumentation for SEC/GPC and detection systems: UV absorption spectrophotometric, diode array UV (DAD), refractive index, evaporative light scattering (ELSD).
Analytical methods for the characterization of materials based on mass spectrometry
Principles of mass spectrometry (MS) and instrumentation: ionization sources, analyzers, detectors, system for data acquisition and processing. “Soft” ionization sources (ESI, MALDI), mass analyzers and their characteristics (resolution, mass accuracy). Low-resolution mass spectrometry. High-resolution mass spectrometry. Tandem mass spectrometry. Interpretation of mass spectra. Hyphenated techniques: LC-MS, LC-MS/MS
Analytical methods for the characterization of inorganic materials based on atomic spectroscopy
Atomic absorption spectroscopy (AAS): outline
Inductively coupled plasma source optical emission spectroscopy (ICP-AES).
Inductively coupled plasma source-mass spectrometry (ICP-MS): outline
Insights into sampling and pre-treatment techniques and preparation of a sample for analysis.
Analytical methods for the morphological characterization and compositional analysis of materials based on electron microscopy techniques
Scanning electron microscopy (SEM) for the characterization of conductive materials. Environmental scanning electron microscopy (ESEM) for the characterization of non-conductive materials: spectroscopy and mapping from energy dispersed X-ray emission (EDX) (ESEM-EDX): qualitative and quantitative compositional information on elements; acquisition and processing of images relating to the distribution of elements within an area (mapping).
Laboratory activities relating to applications of atomic spectroscopy, chromatographic, mass spectrometry and electron microscopy techniques for the characterization of materials:
- SEC/GPC for the dimensional characterization of polymers
- MALDI-MS for the structural characterization of polymers
- Pretreatment of samples by microwave mineralization for screening analysis of metal impurities in materials using ICP-AES
- ESEM-EDX for the morphological characterization of materials and compositional analysis of elements.
Bibliography
Daniel C. Harris, Chimica Analitica Strumentale, terza edizione, Zanichelli, ebook, https://online.universita.zanichelli.it/harris3e/
Teaching methods
Frontal lessons with presentation of the contents by the teacher (5 credits = 40 hours).
Laboratory activities related to applications of techniques covered in frontal lessons (1 CFU = 15 hours)
Assessment methods and criteria
The knowledge acquired and the ability to understand the concepts covered in the frontal lessons are verified through a written exam and an oral exam.
The written exam consists of open questions on all the topics of the program and is subject to an initial evaluation with assignment of a grade. Students complete the writing in an assigned time and space.
The oral exam focuses on the discussion of the written test with the Commission and on other parts of the program that were not covered by the written test. The oral exam will also include the assessment of knowledge relating to the laboratory activities: in particular, the laboratory notebook will be evaluated, drawn up on the basis of the experiences proposed and the learning of the topics covered in the preparatory lessons for carrying out the laboratory exercises.
The Commission assigns a grade to the exam which includes the grade of the written exam and a score given to the reports to be delivered on the laboratory credit.
The final grade will be integrated with that assigned to the "Physical characterization of materials" module to calculate the overall grade of the exam as the arithmetic mean of the two modules.
Will be evaluated:
- learning of the basic concepts and tools of instrumental analytical chemistry for the chemical characterization of materials.
- critical evaluation of instrumental analytical techniques in terms of principles, scope and performance in relation to the characteristics of the materials and the objectives of the analysis
- critical evaluation of the quality parameters of analytical methods
- acquisition of a formally correct language, ability to express the contents clearly, elaboration of links between the different parts of the Course.
Other information
Support activities:
a) Case studies of application of instrumental analytical techniques for the chemical characterization of materials.
b) Screening of illustrative videos of analytical instrumentation as complementary educational tools
It is essential to use the didactic material which is projected in the classroom during the lessons and which is made available online.
The Syllabus of the Course will be illustrated and examined for all that pertains to the following aspects:
-Course contents
- reference texts
- training objectives
- prerequisites
- teaching methods
-learning verification mode
At the end of the illustration, the teachers will take care to verify the correct understanding of the syllabus of the teaching in question.
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