F1AI2_15 Analytical Chemistry II

Faculty of Pharmacy
Spring 2024
Extent and Intensity
2/3/0. 7 credit(s). Type of Completion: zk (examination).
Teacher(s)
doc. RNDr. Bc. Jiří Pazourek, Ph.D. (lecturer)
doc. RNDr. Bc. Jiří Pazourek, Ph.D. (seminar tutor)
Mgr. Hana Pížová, Ph.D. (seminar tutor)
PharmDr. Tereza Padrtová, Ph.D. (seminar tutor)
Mgr. Michaela Kuchynka, Ph.D. (seminar tutor)
Mgr. Hubert Veselý (seminar tutor)
Bc. Gabriela Jelínková (assistant)
Mgr. Tomáš Crha (seminar tutor)
Ing. Klára Odehnalová, Ph.D. (seminar tutor)
doc. PharmDr. Ing. Radka Opatřilová, Ph.D., MBA (seminar tutor)
Guaranteed by
doc. RNDr. Bc. Jiří Pazourek, Ph.D.
Department of Chemical Drugs – Departments – Faculty of Pharmacy
Supplier department: Department of Chemical Drugs – Departments – Faculty of Pharmacy
Timetable
Mon 9:00–10:40 44-056
  • Timetable of Seminar Groups:
F1AI2_15/01: each odd Tuesday 13:00–18:00 44-339, T. Crha, J. Pazourek
F1AI2_15/02: each odd Wednesday 7:30–12:30 44-339, T. Crha
F1AI2_15/03: each odd Wednesday 13:00–18:00 44-339, K. Odehnalová
F1AI2_15/04: each even Tuesday 13:00–18:00 44-339, M. Kuchynka, J. Pazourek
F1AI2_15/05: each even Wednesday 7:30–12:30 44-339, K. Odehnalová
F1AI2_15/06: each even Wednesday 13:00–18:00 44-339, K. Odehnalová
Prerequisites
F1AI1_15 Analytical Chemistry I
3150/F1AI1
Course Enrolment Limitations
The course is also offered to the students of the fields other than those the course is directly associated with.
The capacity limit for the course is 150 student(s).
Current registration and enrolment status: enrolled: 119/150, only registered: 0/150, only registered with preference (fields directly associated with the programme): 0/150
fields of study / plans the course is directly associated with
Course objectives
Objectives: To provide the theoretical and practical knowledge for qualitatively performing chemical and instrumental analysis of inorganic and organic substances including pharmaceuticals, emphasizing the importance of methods e.g. in drug analysis and in studying structural and physico-chemical properties of substances related to their biological effect. Emphasis is placed on shaping the logical thought processes of a pharmacist important for his future professional use. Practical exercises are required to master working habits and students' independent approach to solving analytical problems.
Learning outcomes
After completing the course the student will be able to: - understand the meaning and principles of classical and modern quantitative analytical chemistry - have an overview of methods and practically perform gravimetry, volumetry, photometry, potentiometric titration, HPLC and capillary electrophoresis
Syllabus
  • Lessons:
    1.-2. Quantitative analysis: basic concepts and methods of quantitative analysis. Sample preparation, dissolution of samples. Solutions, expressing their composition, the measurement of volume. Gravimetry, calculations in gravimetry, gravimetric factor, analytical scales and weighing.

    3.- 5. Introduction to volumetric analysis: definition. Standard solutions, primary standards, finding the exact concentration of standard solutions. Types of titrations, titration curve, indications of equivalence point. Acid-base, precipitation, complexometric, redox titrations.
    6.-8. The basics of optical methods. Properties of the electromagnetic radiation: interaction of mass and radiation. The emission, absorption of radiation, fluorimetry, AAS, AES, ICP-AES, change of the direction and speed, optical rotation. ORD. Circular dichroism (CD).
    9.-10. Basic concepts and principles of electroanalytical methods. Direct and indirect methods (titrations). The methods used in pharmaceutical analysis: conductometry, high-frequency conductometry, potentiometry, amperometry (Clark cell), coulometry, voltammetry, polarography, diferential pulse polarography, striping voltammetry.
    11.-13. Introduction to separation methods: Classification, basic principles, examples of applications. Extraction liquid-liquid, SPE. Chromatographic methods (IEC, GC, HPLC, TLC). Typical applications of HPLC
    14. Electromigration methods (CZE, cIEF, cITP, MEKC). Instrumentation, typical applications.
    Laboratory exercise
    1. Gravimetric Determination of iron or a Ferric Salt in the Form of Ferric Oxide
    2. Volumetric determination of an Insoluble Carbonate by Back Titration
    3. Complexometric Determination of Bismuth and Zinc by Stepwise Titration
    4. Spectrophotometric determination of copper with Complexon III / Determination of antipyrine with Fe(3+)
    5. Argentometric determination of halides mixture with potentiometric end-point indication / Alkalimetric determination of phosphoric acid with potentiometric end-point indication
    6. Determination of caffeine in tablets of Acifein by high-performance liquid chromatography (HPLC)
    7. Determination of acetylsalicylic acid (ASA) in tablets of Acifein by capillary zone electrophoresis (CZE)
Literature
    required literature
  • Pazourek J., Kapustíková I., Odehnalová K. Cvičení z analytické chemie 2. Analytická chemie kvantitativní. VFU Brno, 2014. ISBN 978-80-7305-735-0. URL info
  • Karlíček, R. a kolektiv. Analytická chemie pro farmaceuty. Praha, UK, 2005. info
    recommended literature
  • Šmejkal K, Muselík J, Mokrý P. Laboratorní metody experimentální fytochemie. Brno, 2013. ISBN 978-80-7305-649-0. info
  • MZČR. Český lékopis. Praha, 2009. ISBN 978-80-247-2994-7. info
  • Štulík, K a kol. Analytické separační metody. UK Praha, 2004. info
  • Klouda, P. Moderní analytické metody. Nakladatelství P. Klouda Ostrava, 1996. info
  • Churáček, J. a kolektiv. Nové trendy v teorii a instrumentaci vybraných analytických metod. Academia Praha, 1993. info
Teaching methods
oral lessons laboratory exercises
Assessment methods
tests after lectures (continuous) written test (on-line)
Language of instruction
Czech
Further comments (probably available only in Czech)
Study Materials
The course can also be completed outside the examination period.
Teacher's information
https://moodlinka.ics.muni.cz/course/view.php?id=3664
To gain credits, a student must take part in ALL the laboratory
exercises and pass all written exercise tests (or MOODLE tests).
Requirements for examination:
Analytical reactions: types of analytical reactions, requirements for qualitative (proof) and quantitative (determination) analysis. Agent, analyte, sample, matrix.
Protolytic reactions: water as a solvent, definition of pH, calculation of pH of aqueous solutions, weak/strong acids and bases, buffers.
Qualitative chemical analysis: general procedure of qualitative analysis.
Tests for important inorganic cations and anions.
Proof and identification of organic compounds: preliminary tests. Determination of basic physical properties (constants). Elemental analysis. Solubility classes. Tests for oxygen and nitrogen functional groups. Classical and modern methods of identification of organic compounds.
Quantitative analysis: basic terms, method classification. general procedure of quantitative analysis. Calculations and results evaluation. Sample preparation, dissolution of samples. Solutions, expression of solution concentrations, volume measurement.
Gravimetry, analytical balances and weighing, calculations in gravimetry, gravimetry factor.
Volumetry: volumetric solutions, primary standards, determination of precise concentration of volumetric solutions. Indication of the end-point - indicators. Types of titrations, titration curves. Precipitation titrations - the solubility product. Complexometric titrations - stability constants. Principles of volumetric methods - alkalimetry, acidimetry, complexometry, argentometry, redox titrations. Calculations in volumetric analysis - end-point determination.
Instrumental methods - determination with calibration curve.
Optical methods: interaction of mass and radiation, electromagnetic radiation (EMG). Classification of optical methods (radiation absorption/emission, changes of direction, speed and optical rotation of radiation). Principles instrumentation and applications of optical methods in pharmaceutical analysis - molecular and atomic methods, absorption and emisson analysis (UV-VIS, infrared spectroscopy, Raman spectroscopy, AAS, AES, ICP-MS), refractometry, polarimetry, circular dichroism (CD). Nephelometry, turbidimetry. Absorbance, blank sample, spectrum.
Electroanalytical methods: basic terms and principles, redox analytical reactions, redox potential, its measurements, factors affecting the redox potential, electrochemical series of reduction potentials.
Electrochemical methods used in pharmaceutical analysis - potentiometry (type of electrodes incl. ISE), potentiometric titrations, Voltametry - polarography, coulometry, electrogravimetry, conductometry.
Separation methods: classification, basic principles. Extraction - LLC. Chromatographic methods (TLC, HPLC, IEC, GC). Special detectors in chromatographic methods (FID, ECD, MS).
Electromigration methods (CZE, IEF, ITP, HPCE). Detection in electromigration methods. Evaluation of chromatograms - capacity factor k´, efficiency of a column N, HETP, resolution Rs. Evaluation of electroforeogram - electroosmotic flow (EOF), electrophoretic mobility u.
The course is also listed under the following terms Spring 2020, Spring 2021, Spring 2022, Spring 2023, Spring 2025.
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