Unit INSTRUMENTAL ANALYTICAL CHEMISTRY
- Course
- Chemistry
- Study-unit Code
- 55030806
- Curriculum
- In all curricula
- Teacher
- Catia Clementi
- Teachers
-
- Catia Clementi
- Hours
- 47 ore - Catia Clementi
- CFU
- 6
- Course Regulation
- Coorte 2021
- Offered
- 2022/23
- Learning activities
- Caratterizzante
- Area
- Discipline chimiche analitiche e ambientali
- Academic discipline
- CHIM/01
- Type of study-unit
- Obbligatorio (Required)
- Type of learning activities
- Attività formativa monodisciplinare
- Language of instruction
- Italian
- Contents
- Introduction to instrumental analytical chemistry.
Validation of an analytical method and figures of merit. Calibration and calibration methods. Optical spectroscopy. Atomic spectroscopy. UV-Vis spectroscopy. Colorimetry. Chromatography. - Reference texts
- •Teaching material provided by the teacher.
• Universitary texts in analytical chemistry:
- “CHIMICA ANALITICA STRUMENTALE” Skoog, Holler, Crouch. EdiSES
- "CHIMICA ANALITICA QUANTITATIVA".
Daniel C. Harris. ZANICHELLI - Educational objectives
- The main objective of the course is the understanding of the fundamental principles of instrumental analytical chemistry through the learning of analytical methods based on the use of spectroscopic and chromatographic techniques. The potential and the limits of the analytical methodologies desccribed through examples of applications in different fields (environmental, medical, food, industrial) will be highlighted. Methods of processing the analytical data experimentally obtained will be discussed.
- Prerequisites
- For a full and easy understanding of the topics of this course it is important to have good basic knowledge of General Chemistry and Physical Chemistry, optics and electromagnetism
- Teaching methods
- The course is organized in the following way:
- face to face lectures concerning all the topics of the program through PowerPoint presentations;
-exercises concerning the main topics;
- laboratory exercises: three laboratory exercises are planned (about 4 hours each) scheduled in three shifts, to be held in groups, regarding the use of UV-Visible absorption and emission spectroscopy and chromatography for quantitative determination of analytes. - Other information
- Learning verification modality
- The exam includes an oral test and the preparation of lab experience reports:
1) oral exam: it consists of an interview long enough to determine and verify the knowledge level, understanding capability and technical skills achieved by the student on the topics covered during the frontal lectures and the analytical techniques used during the laboratory experiences. It will be tested also the capacity of the student to communicate and present the theoretical contents with an appropriate scientific language and the critical sense acquired by the student in dealing with practical issues
2) laboratory reports: at the end of each laboratory experience, each group must provide a written report containing the experimental procedure followed, the results obtained and their re-elaboration. - Extended program
- 1) Definition of terms used in analytical chemistry (sample, matrix, analyte, chemical interference, measurement, analysis, difference between method, protocol, analytical technique and procedure). Classification of analytical methods in classical and instrumental methods.
2) The choice of the analytical method - figures of merit. Accuracy and precision. Measurement of experimental error. Systematic and random error. Sensitivity. Limit of detection and quantification. Dynamic and linear range. Selectivity. Control charts.
3) Calibration methods. Primary standards, reference materials and certified reference materials. Standard and blank solutions. Calibration line using the least squares method. Standard deviation of slope, intercept, regression and unknown analyte concentration. Correlation coefficient. Determination of lod and loq from repeated measurements on the blank, from the calibration line and from the signal / noise ratio.
Calibration with external standard, internal and standard addition method.
4) SPECTROMETRIC METHODS: Introduction. Wave and corpuscular properties of electromagnetic radiation, interaction electromagnetic radiation and matter (reflection, transmission, refraction, diffraction, absorption, emission), the electromagnetic spectrum, Lambert-beer law. OPTICAL SPECTROSCOPIC METHODS: instrumentation (sources, monochromators, sample compartment, detectors and wavelength selectors) with particular reference to UV-Vis and atomic and molecular spectroscopy
ATOMIC SPECTROSCOPY: instrumentation for absorption, emission and atomic fluorescence. Atomic absorption: sodium spectrum, sources, spectral widening phenomena, temperature effect, methods of introducing solution and solid samples, flame and thermoelectric atomization, description and operation of the two types of atomizers. Instrumentation for atomic absorption.
UV-VIS SPECTROSCOPY. absorption spectroscopy: absorption spectra, double-beam, single-beam and multi-channel spectrophotometers. Spectrophotometer for measurements surface reflection and solid samples, the integrating sphere. Quantitative determinations: Lambert-Beer law and its deviations. Spectrofluorimetry: theoretical aspects and instrumentation. The spectral correction. Quantitative determinations. Colorimetry: theoretical aspects and instrumentation. Color origin. Subtractive and additive colors. The RGB and CLMK system. Hue, saturation and brightness, the CIELab model.
5) The principles of chromatography. Origins and definitions. Classification of chromatographic methods based on the state of aggregation of the mobile and stationary phase, based on the physical mode of contact between the mobile phase and the stationary phase and on the basis of the interactions between solutes and stationary phase. Analytical and preparative chromatography. Chromatographic bands and peaks. The chromatogram, the chromatographic peak and its basic amplitude, retention time and correct retention time, dead time, average migration speed of solutes and mobile phase. The partition coefficient and its relation to the migration speed of solutes. Retention coefficient and its relationship with the speed of migration and with the retention times of solutes. The classical theory of theoretical plates and chromatographic efficiency. Kinetic theory of velocities. Van Deemter's equation. Chromatographic resolution. Optimization of a chromatographic process.
Gas chromatography: definition and field of application, The equipment, The carrier gas, Injectors: split / splitless, on-column and PTV, The gas chromatographic columns: packed and capillary.
High performance liquid chromatography (HPLC): field of application, Block diagram, Solvents for liquid chromatography, degassing, isocratic and gradient HPLC pumps, manual and automatic injectors. HPLC columns: Stationary phase types, Particle size, Particle shape, Porosity. Exclusion Chromatography,
HPLC Detector: Visible UV, DAD, ELSD, MS.
Qualitative and quantitative chemical analysis with chromatographic techniques: Calibration and response factor, Internal Normalization, External Standardization, Addition Method.