Learning objectives
The course aims to provide students with advanced knowledge of the analytical process, the classification of analytical methods and the main instrumental analytical techniques, with particular regard to spectroscopic, separative and coupled analytical techniques. A critical discussion of the principles, performance and fields of applicability of the techniques is emphasized. The aim of the course is also to guide students to a critical evaluation of the experimental results in relation to the performance of instrumental techniques, the field of investigation (qualitative, quantitative or confirmation method) and to the quality parameters of the analytical methods, applying a "problem solving" approach. The concept of validation of analytical methods is defined and the European guidelines for validation are illustrated.
At the end of the course the student is expected to be able to:
- know the principles and the analysis procedures for the characterization of chemical compounds;
- to know the fundamental principles of the methods of instrumental analysis, with the classification of the instrumental analytical techniques, and the relative selection criteria;
- performing stoichiometric calculations and practical operations in relation to the preparation of solutions of known concentration;
- choose and use the best method of separation, purification and analysis of a mixture;
- collect scientific data through laboratory observations and measurements, to elaborate and interpret them;
- carry out the sampling, the preparation of the sample and draw up the documentation of the analysis performed;
- communicate, both in oral and written form, in the context of professional activities and relationships, with a strict respect for the chemical language;
- interacting with other staff on the implementation of procedures and the necessary safety measures in the chemical field;
- undertake academic studies of a higher level with a sufficient degree of autonomy or to continue the professional training;
- work by objectives, in groups or independently;
- adapt to different areas of work and issues;
- to interpret, in an autonomous way, data of technical-scientific literature, especially in the practical-applicative field
Prerequisites
Physics I. Physics II.
Analytical Chemistry and Laboratory of Analytical Chemistry.
Course unit content
Introduction to instrumental analytical methods
Classification of analytical techniques
Criteria for the choice of analytical methods. Development and validation of analytical methods.
Method performance characteristics.
Calibration methods.
Spectroscopic techniques
Molecular Absorption and Fluorescence UV-vis Spectrophotometry.
Molecular Absorption IR Spectrophotometry.
Atomic Absorption Spectrophotometry.
Atomic Emission Spectrophotometry.
Mass Spectrometry.
X-ray Diffraction.
Separation techniques
Theory and application of chromatography. Gas chromatography and liquid chromatography.
Laboratory experiments
Full programme
Introduction to instrumental analytical methods
Classification of analytical techniques
Criteria for the choice of analytical methods. Development and validation of analytical methods.
Method performance characteristics according to European guidelines for the validation of analytical methods: linearity range, detection and quantitation limits, sensitivity, selectivity, accuracy (precision and trueness).
Types of calibration methods: external calibration, internal standardization, standard addition method.
Spectroscopic techniques
Fundamentals of spectrophotometry.
Molecular Absorption and Fluorescence UV-vis Spectrophotometry. The nature of electronic transitions. Instrumentation for molecular absorption UV-vis spectrophotometry: sources, monochromators, detectors. Photodiode array detector. Trasmittance and absorbance. Lambert-Beer law and deviations. Applications to quantitative analysis.
Instrumentation for molecular fluorescence UV-vis spectrophotometry. Fluorescence and phosphorescence. Effect of temperature on the fluorescence quantum yield. Quantitation: relation between the intensity of fluorescence emission of dilute samples and analyte concentration.
Atomic Absorption Spectrophotometry. Atomic spectra. Instrumentation: hollow cathod lamp, atomizers (flame and graphite furnace atomic absorption spectroscopy, hydride generation atomic absorption spectroscopy, Cold vapor atomic absorption spectroscopy). Spectral and non spectral interferences. Background correction systems.
Atomic Emission Spectrophotometry. Instrumentation: ICP source, high-resolution monochromators, detectors.
Molecular Absorption IR Spectrophotometry. Modes of molecular motion; vibrational modes and absorption regions. Factors that influence the frequency of absorption. Characteristic IR absorption frequencies. FT-IR instrumentation: sources, Michelson interferometer, detectors. FT-IR gas analysis. Applications of IR spectroscopy to the characterization of organic compounds.
Mass Spectrometry. Fundamentals. Instrumentation: electron ionization source, chemical ionization source, analyzers (magnetic sector, quadrupoles, ion trap, time-of-flight), detector.
X-ray Diffraction. Fundamentals and instrumentation.
Separation techniques
Theory and application of chromatography. Gas chromatography and liquid chromatography.
Chromatographic parameters. Retention time. Capacity factor. Selectivity factor. Resolution. Band broadening and column efficiency.
Gas chromatography. Gas-solid chromatography (GSC). Gas-liquid chromatography (GLC). Stationary phases for GSC and GLC. Instrumentation: injectors, columns, detectors. Capillary columns. Universal and selective detectors. Gas chromatography-mass spectrometry. Isothermal gas chromatography. Temperature-programmed gas chromatography. Internal standard calibration method for quantitative determinations.
Liquid chromatography (TLC, preparative LC and analytical LC (HPLC)). Mechanisms of separation: adsorption chromatography, partition chromatography, ion chromatography, size-exclusion chromatography. Instrumentation for HPLC: injection valve, columns, pumps, detectors. Isocratic elution, gradient elution.
Bibliography
K.A. Rubinson, J.F. Rubinson, Chimica Analitica Strumentale, Zanichelli, 2002.
Holler, Skoog, Crouch, Chimica Analitica Strumentale, II edizione, EdiSES, 2009.
D.S. Hage, J.D. Carr, Chimica Analitica e Analisi Quantitativa, Piccin, 2012.
Teaching methods
Academic teaching. Interactive teaching. Laboratory experiments.
Academic teaching will be supported by interactive educational paths with the aim of stimulating interest in the subject and comparing different approaches to the topics covered.
Cycles of analytical laboratory experiences will be activated for 1 CFU (15 hours) during which students will be required to apply the most relevant analytical techniques according to the methodological criteria illustrated in the lessons. For each laboratory experience the student will be required to prepare a report in paper format with a discussion of the analytical results.
The teaching materials used in the classroom are uploaded to Elly at the beginning of the course. The slides of the Course are considered an integral part of the teaching material.
Assessment methods and criteria
Learning of the basic concepts and tools of instrumental analytical chemistry. Acquisition of a formally correct language, ability to express contents in a clear and linear way, elaboration of links between the different parts of the course. Critical evaluation of instrumental analytical techniques and correct classification of analytical methods. Critical evaluation of the quality parameters of the methods.
The acquired knowledge and the ability to understand the concepts treated are verified through a written and oral examination.
The acquired knowledge and the ability to understand the concepts treated are verified through a written test and an oral test with a summative assessment.
The written test, with an open answer, has a duration of 2 hours. The written test is evaluated with a scale of 0-30. The vote of the written test is communicated within two days following the test, by publication on Elly.
In the oral examination, the student is evaluated on the basic concepts of instrumental analytical chemistry, on the acquisition of a formally correct language, and on the definition of relationships between the different parts of the course. A critical evaluation of instrumental analytical techniques and a correct classification of analytical methods is also required, with a critical evaluation of the quality parameters of the methods. The activity carried out in the laboratory will also be examined through an assessment of the lab report and through learning of the concepts related to the experiments. The lab report is to be delivered at least ten days before the date of the oral exam; please note that the last deadline for the report delivery is 31st July of the course attendance year, also in case of enrollment to subsequent exam sessions.
The oral exam is evaluated on a scale of 0-30. The oral test vote is communicated immediately at the end of the test itself.
The final mark is obtained by taking into account the mark of the written test and the oral exam (both in thirtieths).
Please note that online registration is mandatory both in the case of a written test and in the case of an oral exam.
Other information
Illustration of case studies of instrumental analytical techniques in the food, environmental, biological and forensic fields.
