Course code:
260S2
Course name:
Combined Technics of Instrumental Analysis

Academic year:

2023/2024.

Attendance requirements:

There are no requirements.

ECTS:

9

Study level:

graduate academic studies

Study program:

Environmental Chemistry: 1. year, winter semester, elective (E52S2) course

Teacher:

Vele V. Tešević, Ph.D.
full professor, Faculty of Chemistry, Studentski trg 12-16, Beograd

Assistant:

Gordana B. Krstić, Ph.D.
assistant professor, Faculty of Chemistry, Studentski trg 12-16, Beograd

Hours of instruction:

Weekly: four hours of lectures + two hours of exercises + three hours of labwork (4+2+3)

Goals:

The objective of this course is to introduce techniques and methods, which are used to analyze environmental samples; overcome sample preparation and application of chromatographic techniques with proper selection of suitable detector for chromatographic analysis; application of tandem (MS/MS) and multistage mass spectrometry (MSn).

Outcome:

Students will be trained to prepare samples for various instrumental analysis. They will be able to independently design experiments, select appropriate devices and techniques and perform a detailed analysis of environmental samples.

Teaching methods:

Lectures, theoretical exercises, labwork, colloquia and semmester papers.

Extracurricular activities:

Guest lectures.

Coursebooks:

  1. Vele Tešević: Osnove masene spektrometrije organskih jedinjenja
  2. Slobodan Milosavljević: Strukturne instrumentalne metode

Additional material:

  Course activities and grading method

Lectures:

0 points (4 hours a week)

Syllabus:

  1. Environmental samples and methods for their preparation (liquid-liquid extraction, derivatization, headspace, SPE, QuEChERS, MEPS).
  2. Chromatographic techniques and their principles (HPTLC, HPLC, UPLC, GC, CG/CG and IEC).
  3. Types of detectors in chromatographic analysis (densitometer, UV-Vis, DAD, ELSD, FID, FPD, NPD, RI, FTIR, MS, etc.).
  4. Types of ion sources (EI, CI, FD, FAB, SIMS, PD, DART, MALDI, SELDI, ESI, APCI, APPI, CID / CAD) and analyzers (B, E, Q, ion trap (IT), TOF, ICR, Orbitrap) in mass spectrometry.
  5. Tandem (MS/MS) and multistage mass spectrometry (MSn).
  6. Qualitative and quantitative analysis, validation and verification of quantitative methods.
  7. MS/MS experiments of qualitative and quantitative targeted analysis (MRM, SRM, product scan, daughter scan and neutral loss scan).
  8. Combined instrumental analysis techniques (HPTLC/MS, GC/MS, GC/GC/MS, GC/MS/MS, LC/MS, LC/MS/MS, LC/MSn).
  9. Combined Instrumental methods in chemical weapons analysis.

Exercises:

10 points (2 hours a week)

Syllabus:

  1. Qualitative analysis, processing of EI-MS spectra and identification of analyzed compounds by comparing recorded spectra with spectra from the library (NIST and WILEY) using the AMDIS program.
  2. Quantitative analysis, validation and verification of methods.
  3. Quantitative analysis, results processing and measurement uncertainty estimation.

Labwork:

20 points (3 hours a week)

Syllabus:

  1. Liquid-liquid extraction sample preparation.
  2. Derivative preparation of samples for gas and gas-mass chromatography.
  3. Headspace and SPE sample preparation.
  4. Application of MEPS in sample preparation.
  5. Chromatographic analysis of prepared samples by high performance thin layer chromatography (HPTLC).
  6. Chromatographic analysis of prepared samples by gas and gas-mass chromatography (CG/MS).
  7. Chromatographic analysis of prepared samples by high performance liquid chromatography (HPLC/MS).

Semester papers:

20 points

Colloquia:

20 points

Oral exam:

30 points