84748 - Analitical Chemistry 3

Learning outcomes

At the end of the course the student acquires theoretical and instrumental fundamentals to use analytical technologies and methodologies of separation science, spectrophotometry and mass spectrometry. The student will be able to choose most suited methodologies to face simple problems of analytical chemistry, to find in them the critical aspects, and to show how to optimize quality of the analytical results thereby obtained.

Course contents

Recommended Background:

To fully benefit from the lectures and perform successfully on the final exam, students are expected to have a solid understanding of Analytical Chemistry, Physical Chemistry, General Chemistry, Organic Chemistry, Physics, and Mathematics, as acquired in previous semesters of the Chemistry degree program (course code 84748). For non-native Italian speakers, C1-level proficiency in Italian is recommended.

 

This Course is divided into two modules, totaling 8 ECTS credits:

• Module 1: Instrumental Analytical Chemistry (6 ECTS) — delivered through in-class lectures.

• Module 2: Analytical Chemistry Laboratory III (2 ECTS) — primarily conducted in the laboratory, with occasional classroom sessions to introduce the theoretical foundations of the experiments.

Module 1 – Instrumental Analytical Chemistry (6 ECTS)

• Course overview and introduction.

• Principles of analytical spectroscopy: absorption and emission spectra (atomic and molecular); qualitative and quantitative analysis; derivation and limitations of the Lambert–Beer law; absorbance measurements and associated errors; emission spectroscopy: photoluminescence and chemiluminescence.

• Instrumentation in analytical spectroscopy: light sources; wavelength selectors (filters, monochromators with prisms and gratings); spectral bandwidth; detectors (phototubes, photomultiplier tubes, diode arrays); single- and double-beam spectrophotometers; noise reduction techniques (e.g., chopper systems); spectrophotometric detectors for liquid chromatography.

• Atomic spectroscopy fundamentals: light sources (e.g., hollow cathode lamps), atomizers (flame, graphite furnace, plasma), background correction methods.

• Separation techniques: chromatographic principles; peak properties; retention time; theoretical plates; separation efficiency and influencing factors; efficiency measurements; capacity factor, selectivity, and resolution; Van Deemter equation and its experimental implications; nonlinearity in distribution isotherms.

• Gas chromatography (GC): packed and capillary columns; stationary phases; temperature programming; sample injection systems; GC detectors.

• Liquid chromatography (LC, HPLC): operational modes; pump and injector systems; stationary phases; normal-phase and reverse-phase LC; mobile phase gradients; criteria for choosing appropriate LC methods; LC detectors.

• Mass spectrometry (MS): basic principles and instrumentation; ionization sources (electron impact, chemical ionization, electrospray ionization [ESI], fast atom bombardment [FAB], MALDI); mass analyzers (magnetic sector, quadrupole, time-of-flight).

Module 2 – Analytical Chemistry Laboratory III (2 ECTS)

• Spectroscopic techniques: UV-Vis absorption, atomic absorption for quantifying analytes in complex real matrices; optimization of instrumental parameters; definition of analytical protocols; instrument operation; data acquisition and processing.

• Separation techniques:

  • HPLC analysis: reverse-phase, size-exclusion (SEC), and ion-exchange chromatography; instrument setup; method development and optimization; evaluation of separation performance; quantitative analysis via HPLC: method optimization, data acquisition, and processing.

  • GC analysis: application to quantitative analysis in complex matrices; sample preparation; instrument operation; data acquisition and interpretation.

• Complex sample analysis: sample digestion techniques; calibration methods for evaluating matrix effects; comparative assessment of different techniques for quantitative analysis in complex matrices.

• Indirect protein quantification methods: application of the Bradford assay to determine the protein concentration of unknown samples.

• Miniaturized spectrophotometric approaches: use of microplate readers, microtiter plates, and automated micropipettes for quantitative determinations.

 

Readings/Bibliography

• D. C. Harris, Quantitative Chemical Analysis, Second Italian Edition, Zanichelli Ed., Bologna, 2005 (*)

• Skoog, West, Holler, Crouch, Fundamentals of Analytical Chemistry, Second Edition, EdiSES srl, Naples, 2005

(*) Primary reference textbook

Students are required to use either the first or the second textbook as a reference; one of the two is essential to successfully pass the exam.

Teaching methods

Module 1: this module consists of 48 hours of in-person, classroom-based lectures. All sessions are recorded using Panopto and made available to students via the Virtuale platform. Remote attendance is permitted only in the event of an emergency and must be authorized by the University or the Department.The instructional materials presented during the lectures are essential for full participation and comprehension. These materials are uploaded to Virtuale prior to the start of the course, with a formal announcement made to students through the Announcements tool on Virtuale. Additional multimedia resources available online may also be shared via Microsoft Teams throughout the course.

Module 2: this module consists of 32 hours of laboratory instruction. Attendance at the preliminary in-class lectures is mandatory, as they introduce the experimental methods, laboratory protocols, data analysis procedures, and the preparation of technical reports. Instructional materials for these sessions are provided in electronic format and uploaded to Virtuale before the course begins, with notice given via the Announcements tool on Virtuale. Laboratory manuals, including detailed descriptions of the protocols, are also made available in advance of each scheduled laboratory session. Data recording spreadsheets are provided through Virtuale to facilitate data entry, analysis, and the calculation of quantitative results. During the laboratory sessions, both the manuals and data processing spreadsheets may be updated in response to experimental outcomes and specific learning needs.

Assessment methods

It is strongly recommended that students take the final examination for this course only after successfully completing the courses “Analytical Chemistry 1” and “Analytical Chemistry 2” as part of the Chemistry degree program (course code 84748). To be eligible to take the final exam, students must have attended the lectures for Module 1, preferably in person or, alternatively, by viewing the recorded sessions, and must have obtained the attendance signature for Module 2, which is mandatory.

The final examination consists of an ORAL assessment covering all topics from the course syllabus, aimed at verifying the student’s comprehensive knowledge of the subject matter.

Examinations are conducted in pairs, with a two-member examination committee. One committee member examines the candidate on the content of Module 1, while the other focuses on Module 2. Each candidate is evaluated for approximately 15 minutes by each examiner, for a total exam duration of approximately 30 minutes per student.

If a member of the committee determines that the candidate’s level of preparation is inadequate during their portion of the exam, the candidate may be invited to withdraw from the session.

Upon completion of the assessments, the committee will meet to assign a grade on a 30-point scale, based on the following criteria:

• 18–23 points: Minimal to sufficient knowledge of the subject; may include significant errors.

• 24–26 points: Fair to good understanding; some minor inaccuracies.

• 27–29 points: Good to very good knowledge; minor imperfections and/or presentation flaws.

• 30–30L (“cum laude”): Excellent to outstanding knowledge; thorough and articulate responses with minimal or no imperfections. Honors (“cum laude”) is awarded for clearly exceptional performance.

Following the grade proposal, the committee may ask students to provide a self-evaluation of their performance. If necessary, the committee may engage in a discussion with the candidates regarding any discrepancies between the proposed grade and the self-assessment.

Special Examination Conditions for Module 1: for students who have attended Module 1 during the first semester but have not yet completed or received the attendance signature for Module 2, there is an option to take the Module 1 exam during the winter examination session (first semester only). If the Module 1 exam is passed, and the student subsequently obtains the required attendance signature for Module 2, they must complete the Module 2 exam during the summer session of the same academic year. In this case, the Module 2 exam will be administered in written form, with open-ended questions covering the entire Module 2 syllabus. The final course grade will be determined by the examination committee based on the weighted average of the two individual exam scores.

Teaching tools

Module 1: Instruction is supported by a PC with large-screen projection, with Microsoft PowerPoint slides made available on the Virtuale platform. Microsoft Teams may be used for online teaching only if authorized by the University or the Department. All lectures are recorded using Panopto and made accessible via Virtuale.

Module 2: Instruction is supported by a PC with large-screen projection, with Microsoft PowerPoint slides made available on Virtuale. Microsoft Teams may be used for online delivery in cases of official authorization by the University or Department. When applicable, lectures may be recorded with Panopto and shared via Virtuale. Laboratory manuals (Word format) and data spreadsheets (Excel format) are provided to students in advance via Virtuale, supporting laboratory preparation, data acquisition, and analysis.

 

Students with Specific Learning Disorders (SLD) or temporary or permanent disabilities are strongly encouraged to contact the University’s support office in advance (https://site.unibo.it/studenti-con-disabilita-e-dsa/it). The office will work with the student to propose any appropriate accommodations. All accommodation requests must be submitted to the course instructor at least 15 days in advance and will be evaluated in relation to the Learning Objectives of the Course.

Office hours

See the website of Pierluigi Reschiglian

See the website of Barbara Roda