ANALYTICAL CHEMISTRY AND INSTRUMENTAL
Learning outcomes of the course unit
The course aims to provide students with a thorough knowledge of major instrumental analytical techniques, including spectroscopic techniques, separation techniques, hyphenated techniques and electroanalytical techniques. A critical discussion of equipments, procedures and interpretation of test results is emphasised.
Physics I. Physics II. Analytical Chemistry and Laboratory of Analytical Chemistry.
Course contents summary
Introduction to instrumental analytical methods.
Classification of analytical techniques.
The laboratory process: pre-analytical, analytical and post-analytical phases of testing. Criteria for the choice of analytical methods. Development and validation of analytical methods. Method performance characteristics. Calibration methods.
Molecular Absorption and Fluorescence UV-vis Spectrophotometry.
Molecular Absorption IR Spectrophotometry.
Atomic Absorption Spectrophotometry.
Atomic Emission Spectrophotometry.
Separation techniques. Theory and application of chromatography. Gas chromatography and liquid chromatography.
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.
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. Effect of ring substituents on the fluorescence spectra of substituted benzene derivatives. 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, atmospheric pressure ionization sources; analyzers (magnetic sector, quadrupoles, ion trap, time-of-flight), detector.
Theory and application of chromatography. Gas chromatography and liquid chromatography.
Chromatographic parameters. Retention time. Capacity factor. Selectivity factor. Resolution. Column efficiency.
Gas chromatography. Gas-solid chromatography (GSC). Gas-liquid chromatography (GLC). Stationary phases for GSC and GLC. Isothermal gas chromatography. Temperature-programmed gas chromatography.
Instrumentation: injectors, columns, detectors. Capillary columns. Universal and selective detectors. Gas chromatography-mass spectrometry. 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. HPLC-MS.
Qualitative and quantitative analysis in GC and HPLC.
K.A. Rubinson, J.F. Rubinson, Chimica Analitica Strumentale, Zanichelli, 2002.
Holler, Skoog, Crouch, Chimica Analitica Strumentale, II edizione, EdiSES, 2009
Lectures. Interactive teaching. Laboratory experiments.
Teaching activities will involve frontal lessons; if COVID-19 emergency will persist, also remote modality will be involved.
To promote active participation in the course, the lectures will be accompanied by interactive educational paths using resources available on Elly.
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 after the corresponding lessons have been carried out. 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 written test and the oral test will contribute in equal measure to the determination of the final grade.
Please note that online registration is mandatory both in the case of a written test and in the case of an oral exam.
If it is necessary to integrate the execution of the examinations with the remote modality due to the persistence of the health emergency, we will proceed as follows:
- oral tests (in person/remotely);
- written tests (in person/remotely).
Illustration of case studies of instrumental analytical techniques in the
food, environmental, biological and forensic fields.