Analytical Chemistry

1. Sample pretreatment 1.1 Sampling. 1.2. Sample treatment: pros and cons. 1.3. Extraction techniques. - classification - liquid-liquid - solid-liquid (Soxhlet, pressurized solvente extraction, subcritical water extraction, supercritical fluid extraction) - hybrid (matrix solid phase dispersion, QuEChERS) - solid phase extraction (SPE on cartridge, disk-SPE, dispersive-SPE, magnetic-SPE) - miniaturization - carbon nanomaterials as sorbents for SPE - neoteric solvents (ionic liquids, (deep) eutectic solvents) 2. Validazione di un metodo 2.1 Recovery, precision and accuracy 2.2 Limit of detection,limit of quantitation, etc. 2.3 Sensitivity 2.4 Selectivity and carry over 2.5 Evaluation of matrix effect 2.6 Least squares method 2.7 External calibration 2.8 Internal standard: requirements 2.9 Internal calibration 3. Standard addition method Practical laboratory exercises: validation of a SPE-HPLC-UV method for the analysis of non-steroidal anti-inflammatory drugs in water samples Numerical exercises in the classroom: Calculation of recoveries and precision; application of the least squares method to construct the calibration line; sensitivity; calculation of LOD and LOQ.

Prerequisites include fundamentals of basic analytical chemistry, chromatography (number of theoretical plates, selectivity, peak symmetry, etc.),and of the main chromatographic techniques (adsorption, partition, etc.).

The professor has made available all the teaching material (handouts and power point presentations) used during the course on e-learning platform (require password to the professor). Recommended Books: - Marco Grotti, Francesco Ardini. Il Laboratorio di Chimica Analitica. Concetti di base ed esercizi svolti. EdiSES, 2022. ISBN 978 88 3623068 6 - James W. Robinson, Eileen M. Skelly Frame, George M. Frame II. Chimica Analitica Strumentale_ Un’introduzione_ Piccin, 2023. ISBN 978-88-299-3226-9 - Holler, Skoog, Crouch, Chimica Analitica Strumentale, II edizione, EdiSES, 2009. ISBN 9788879593427 - Statistics and Chemometrics for Analytical Chemistry Copertina flessibile – 27 maggio 2018. Edizione Inglese di James N. Miller. ISBN 978 1 292 18671 9

Attendance is optional for lectures and seminars, but compulsory for laboratory exercises.

To pass the exam, mark has to be not less than 18/30. The student must prove that he has acquired sufficient knowledge of both chromatographic and mass spectrometric techniques. To achieve a score of 30/30 cum laude, the student must master all topics covered during the course, being able to link them in a logical and consistent way. Besides the global preparation level, the final mark will be formulated assessing the following elements: logic followed by the student in solving questions, technical language and oral presentation, adequacy of the proposed solution in relation to the skills acquired by the student at the end of the course.

References (.edu) are cited in the handouts uploaded on e-learning

Teaching activity is organized in lectures, seminars, flipped teaching, laboratory exercises and preparation of reports. All teaching material (power point presentations, handouts, explanation sheets of laboratory exercises) used during the course by the teacher is immediately available by the student on the e-learning platform, especially to facilitate working students.