87822 - Industrial Analytical Chemistry with Laboratory M

Learning outcomes

The course is aimed to acquire the capability, based on the characteristics of the analyte, matrix and availability of the sample, to identify the appropriate instrumentation for the design of an analytical procedure scheme starting from appropriate plans of sampling, also using the appropriate technical regulations. The students will also have acquired the ability to evaluate the quality of an analytical or industrial process on the basis of statistical tests and control charts.

Course contents

Learning Objectives

Knowledge and Comprehension

At the end of the course, students will know:

• statistical methods to evaluate results given by multiple operators
• how to do the quality control of processes
• easy procedures to design experiments
  
• principles and instrumental arrangements of electrochemical and spectroscopic techniques, also hyphenated
• principles and instrumental arrangements of surface analysis
• operating principles of electrocemical sensors

At the end of the course, students will have understood:

• the role of statistical procedures in the management and control of analytical and industrial analytical processes
• issues related to the determination of trace and ultra-trace level analytes, analysis
• the relationship between energy levels of a specific analyte and the desired response
• the relationship between the mass transfer and the electrochemical response of an analyte

Skills and Competences

At the end of the course the student will be able to:

• evaluate the analytical results produced by more than two operators
• build and use control curves to evaluate the quality of  an analytical process
• start and manage small and medium instrumentation (atomic spectroscopy, electrochemical workstations)
• identify the correct procedures and techniques to detect the interferences and the limit of detection (LOD)
  
• knowing how to design an analytical procedure appropriate for the determination of one or more analytes in moderately complex matrices, also by exploiting the related technical regulations.

Topics of the course

Control charts, sampling in industrial environments.

Statistical methods for analytical chemistry and industrial processes:

Analysis of variance (ANOVA). Basic elements of experimental design (DOE).

Spectroscopy and spectrometry:

Atomic emission spectrometry techniques: plasma.

Overview of surface analysis and X-ray analysis methods. X-ray - matter interaction. Overview on X-ray absorption and fluorescence spectroscopy, photoelectron spectroscopy, X-ray diffraction of powders. X-ray tube. Industrial applications of X-ray analysis techniques.

ICP-MS, GC-MS and SIMS interfaced.

Reflection and Refraction of light. Total internal reflection and optical fibers. Evanescent wave. Attenuated total reflectance. Raman spectrometry.

Fundamentals of electroanalytics and electrochemical sensors:

Electron transfer. Mass transport (diffusion, migration and convection). Controlled potential techniques (chronoamperometry, chronocolumbometry, voltammetric techniques).

Techniques for the analysis of trace and ultra-trace elements (anodic, cathodic and potentiometric stripping)

Electrodes modified for sensor applications. Amperometric sensors and biosensors.

Introduction to electrochemical energy storage devices:

Batteries and supercapacitors.

Laboratory and practical activities

The course includes various laboratory experiments and classroom/laboratory exercises carried out in groups. In these experiments the use of different instruments is envisaged, allowing the understanding of the concept of the analytical approach: electrochemical and spectroscopic methods on real samples followed by statistical analyses. The experiments contain elements of all three individual course modules.

PRE-REQUIREMENTS OF KNOWLEDGE AND SKILLS TO FOLLOW THE COURSE

In general, the knowledge and skills acquired in the following courses of a first level degree are required: Mathematics, Physics, Analytical Chemistry and Instrumental Analytical Chemistry.

In particular, students must:

• be able to graphically represent and mathematically derive linear calibration curves.
• know how to apply the method of the calibration curve and standard additions for quantitative determinations in instrumental analysis.
• be able to prepare solutions of known titre at low concentrations with adequate precision
• have acquired a certain competence in the use of simple analytical instruments
• possess elementary notions of optics and algebra
• have developed a certain competence in the use of simple analytical instrumentation

Readings/Bibliography

There are numerous texts, many of which are available in university libraries, which deal with the contents of the course with high competence and completeness.

The student may find it useful to consult those reported in the following list.

Recommended texts:

1. J.C. Miller and J.N. Miller, Statistics and Chemometrics for Analytical Chemistry, 6^th ed., Prentice Hall (UK), 2010
2. M.Castino, E. Roletto, Statistica applicata. Trattamento dei dati per studenti universitari, ricercatori e tecnici. Piccin, 1999 (ISBN: 9788829909353)
3. D.A. Skoog, D.M. West, F.J. Holler, S.R. Crouch, Chimica Analitica Strumentale, III Ed., Edises, 2009 (ISBN:9788879593427).
4. K. A. Rubinson, J. F. Rubinson, Chimica Analitica Strumentale, Zanichelli, 2002
5. P.M.S. Monk "Fundamentals of Electroanalytical Chemistry" J. Wiley & Sons, New York, 2002.

On specific topics, in-depth materials will be provided by the teachers, via the UniBo Virtual platform.

Teaching methods

A series of frontal lessons (individual learning) and three laboratory experiences (group and individual work) are foreseen.

Attendance at the laboratory is compulsory and will be evidenced by signature. In the event of unavailability, even if only partial, of a student for a laboratory experience, the course teachers must be contacted immediately to identify an alternative date or laboratory activity. A calendar with dates for individual laboratory group experiments will be provided during the first two weeks of teaching.

In consideration of the types of activities and teaching methods adopted, the attendance of the laboratory activities requires that all students must attend modules 1 and 2 to be carried out in e-learning mode [link], while Module 3 on safety and health is to be attened in class. Information on dates and methods of attendance of module 3 can be consulted in the appropriate section on the website of the degree programme.

Assessment methods

The assessment of learning consists in a final written exam, to which the vote of the laboratory will be added.

The laboratory vote will consist of:

A report per group for one of the experiments carried out, randomly assigned by the course teachers, maximum four pages (50% of the laboratory mark, delivery deadline before the end of the course.

Individual quiz (5 multiple choice questions) relating to the practical aspects of all three experiences carried out in the laboratory (50% of the laboratory mark, given before the end of the course).

The written exam is made of: a) multiple choice questions or true/false questions; b) an open answer question. The test contains elements of all three individual teaching modules. The duration of the written exam is 2 hours. During the individual laboratory quiz and during the written exam, the use of textbooks, mobile phones and lecture notes (or slides) is expressiy forbidden. The material on which to prepare the answers (protocol sheets, paper, etc.) will be made available by the teachers.

It is possibile to refuse a positive grade only twice.

Teaching tools

The frontal lessons will be supported by multimedia tools. The exercises and laboratory tests will be supported by materials made available online on the UniBo platform "Virtuale". Access to the classrooms is such as to allow students with disabilities to assess usability and promptly request adaptations.

Office hours

See the website of Andreas Stephan Lesch

See the website of Barbara Ballarin

See the website of Marco Giorgetti