B4995 - Industrial Analytical Chemistry with Laboratory

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 understanding

At the end of the course, students will know:

• Statistical methods for the evaluation of results provided by multiple operators.

• The methods for controlling the quality of processes.

• Simple procedures for experimental design.

• The principles and instrumental configurations of electrochemical and spectroscopic techniques, also in combined modes.

• The operating principles of electrochemical 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.

• The issues related to the determination of analytes at trace and ultratrace levels.

• The relationship between mass transport in solution and the electrochemical response of an analyte.

Skills and Competences

At the end of the course, students will be able to:

• Evaluate analytical results produced by more than two operators or groups.

• Construct and use control charts for the evaluation of the quality of an analytical process.

• Start up and manage small and medium-sized instrumentation (atomic spectrometry, electrochemical stations).

• Identify the correct procedures and techniques for controlling interferences and the detection limit.

• Design an appropriate analytical procedure for the determination of one or more analytes in matrices of moderate complexity, also by making use of technical standards.

Course topics

Statistical methods for analytical chemistry and industrial processes:

Analysis of Variance (ANOVA). Basic elements of experimental design (DOE). Control charts. (Module 1)

Spectroscopy and spectrometry:

Atomic spectrometry techniques in absorption and emission. Flame, graphite furnace, plasma. (Module 1)

ICP-MS, GC-MS and SIMS interfaces. (Module 1)

Reflection and refraction of light. Total internal reflection and optical fibres. Evanescent wave. Attenuated total reflectance. Raman spectrometry. (Module 1)

Sampling:

Sampling theory. Sampling in industrial environments. (Module 2)

Fundamentals of electroanalysis and electrochemical sensors:

Charge transfer. Ion-selective electrodes (ISE): applications in industrial matrices. (Module 2)

Electron transfer. Mass transport (diffusion, migration and convection). Controlled-potential techniques (chronoamperometry, chronocoulometry, voltammetric techniques). (Module 2)

Techniques for the analysis of trace and ultratrace elements (anodic, cathodic and potentiometric stripping). (Module 2)

Modified electrodes for sensor applications. Amperometric sensors and biosensors. (Module 2)

Laboratory and exercise activities

The course includes several laboratory experiences and classroom/laboratory exercises carried out in groups. These activities involve the use of different types of instrumentation, allowing students to understand the concept of an analytical approach: electrochemical and spectroscopic methods on real samples followed by statistical analyses.

The laboratory experiences contain elements from both individual modules of the course. For each experience, a detailed procedure will be made available on the UniBo Virtual platform, accompanied by several questions to support the preparation of the activity. Upon entering the laboratory, each group must correctly answer at least one question related to the procedure, in order to demonstrate adequate preparation for the planned activities. For example, if a group is unable to indicate which analyte must be determined, within which concentration range and in which matrix, it will not be admitted to the laboratory and the activity will be postponed to a later date, which must be agreed upon by the group according to the availability of the instruments on the dates assigned for the course.

KNOWLEDGE AND SKILLS REQUIREMENTS TO ATTEND THE COURSE

In general, the knowledge and skills acquired in the first-cycle degree courses in Mathematics, Physics, Analytical Chemistry and Instrumental Analytical Chemistry are required.

In particular, students must:

• Be able to graphically represent and mathematically derive linear calibration curves.

• Know and be able to apply the calibration curve method and the standard addition method for quantitative determination in instrumental analysis.

• Be able to prepare solutions with known concentration at low concentration levels with adequate precision.

• Possess basic knowledge of optics and algebra.

• Have acquired a reasonable competence in the use of simple analytical instrumentation.

Readings/Bibliography

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

Students may find it useful to consult those listed in the following list:

Recommended textbooks:

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

For specific topics, in-depth study materials will be provided by the lecturers through the UniBo Virtuale platform.

Teaching methods

A series of lectures (individual learning), exercises (individual learning and group work), and laboratory experiences (group and individual work) are planned.

Attendance at the laboratory is mandatory. Attendance will be verified by signature. In the event of unavailability, even if only partial, of a student for a laboratory experience, the lecturers must be contacted immediately in order to identify an alternative date or an alternative laboratory activity. A schedule with the dates of the individual experiments for the laboratory groups will be provided during the first two weeks of the course.

Considering the types of activities and teaching methods adopted, attendance of this educational activity requires all students to complete Modules 1 and 2 in e-learning mode [https://www.unibo.it/it/servizi-e-opportunita/salute-e-assistenza/salute-e-sicurezza/sicurezza-e-salute-nei-luoghi-di-studio-e-tirocinio ] and to participate in Module 3 of specific training on safety and health in study environments. Information regarding the dates and methods of attendance for Module 3 can be consulted in the dedicated section of the degree programme website.

Assessment methods

The assessment of learning takes place through a final written exam, to which the evaluation of the laboratory activity is added (between -2 and +2).

The laboratory grade consists of:

• GROUP REPORTS, which contain, for each experience, the collected experimental data, the processing and analysis of the experimental data, and the main observations. The overall weight of the reports in the laboratory grade is 60%. The three individual reports must be submitted through the Virtuale platform within two working days from the completion of the respective experiment.

• FINAL GROUP REPORT on one of the performed experiences, randomly assigned by the course lecturers. The final group report has a weight of 40% in the laboratory grade. Important: a limited, explicitly declared at the end of the report, and non-substantial use of AI is permitted for support activities (allowed for summaries and reformulations). Substantial use of AI for the preparation of the report is not permitted, particularly with regard to the structure of the report, calculations and data processing, the creation of graphs and tables, as well as the formulation of conclusions.

The written exam consists of:
a) multiple-choice or true/false questions;
b) specific questions on the laboratory experiences;
c) an open-ended question.

The exam includes elements from both modules of the course. The duration of the written exam is 2 hours and 30 minutes.

During the exam, the use of textbooks, mobile phones, smartwatches, digital note-taking devices, or teaching materials (slides or personal notes) is not permitted.

The use of a non-programmable calculator, non-erasable pens, and a ruler is permitted.

The material necessary for carrying out the exam (protocol sheets, graph paper, etc.) will be provided by the lecturers.

Regarding the written exam, the use of AI is prohibited. Any use constitutes a violation of academic integrity.

It is possible to reject up to a maximum of two passing grades.

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.

Students with learning disorders and\or temporary or permanent disabilities: please, contact the office responsible (https://site.unibo.it/studenti-con-disabilita-e-dsa/en/for-students) as soon as possible so that they can propose acceptable adjustments. The request for adaptation must be submitted in advance (15 days before the exam date) to the lecturer, who will assess the appropriateness of the adjustments, taking into account the teaching objectives.

Office hours

See the website of Andreas Stephan Lesch

See the website of Barbara Ballarin