Syllabus – Instrumental methods

Introduction to instrumental methods

Instrumental methods, their advantages, drawbacks, classification of instrumental methods, their application in qualitative and quantitative analysis.

Optical methods

Basic optical methods, interaction of radiation with particulate matter, classification of optical methods, their principles and scope, fundamentals of luminescence analysis, practical use of optical methods.
Spectrophotometry in UV spectral region, types of electron transfer, light absorption of organic compounds, absorption spectrum, absorption band, absorption coefficient, double-beam spectrophotometers, diode-array detector, analytical applications – identification, purity of substances, quantitative assay, calibration curve, analysis of multi-component systems.
Infra-red spectrophotometry, types of vibrations, characteristic vibrations of functional groups, absorption spectrum, absorption bands, instrumentation, measuring techniques, analytical applications – interpretation of IR spectra, identification, purity, structure of organic compounds.
Flame photometry, refractometry, polarimetry, principles, and analytical applications.

Electroanalytical methods

Basic electroanalytical methods, their classification and principles. Potentiometry, principles, instrumentation, selection of electrode system, ion-selective electrodes, potentiometric titrations and their evaluation, analytical applications. Conductimetry, principles, conductimetric titrations and other applications.
Voltammetry and polarography, principles, instrumentation, qualitative and quantitative analysis.

Radioanalytical methods

Basic radioanalytical methods, their classification, principles, applications.

Separation methods

Basic separation methods, classification according to the principle of separation. Chromatographic methods and their classification.
Gas chromatography, instrumentation, analytical applications.
Liquid chromatography in planar and packed-bed arrangement. High-performance liquid chromatography (HPLC). Thin-layer chromatography (TLC, HPTLC). Paper chromatography. Instrumentation and analytical applications.

INSTRUMENTAL METHODS - LABORATORY TRAINING PROGRAMME

1)    Acidimetric titration with potentiometric end-point indication. Calibration of the electrode system. Determination of sodium tetraborate in solid sample. Graphical evaluation and end-point estimation according to Hahn method. Graphical evaluation and end-point estimation according to Hahn method.

2)    Dichromatometric titration with potentiometric end-point indication. Determination of % content of ferrous salt in a solid sample.

3)    Argentometric titration with potentiometric end-point indication. Determination of Cl^-, Br^-and I^- in a mixture.

4)    Spectrophotometric assay of sulphosalicylic acid in a solution. Finding absorption maximum, optimum amount of reagent. Mesurement of calibration curve, graphical and statistical evaluation.

5)    Spectrophotometric assay of cupric salts in the form of complex with EDTA. Preparation of calibration solutions, evaluation of calibration curve. Determination of Cu²⁺ content in a solid sample.

6)    Extraction - spectrophotometric assay of ferric salts. Formation of the complex with 8-quinolinol and its extraction into chloroform. Preparation of calibration solutions, evaluation of calibration curve. Determination of Fe(III) content in a test solution.

7)    Identification of organic compound by the measurement of the melting point of derivative.

8)    Thin-layer chromatography (TLC). Derivatization for separation purposes, detection, evaluation of chromatograms. Identification of an unknown organic compound.

9)    UV spectrophotometry. Measurement of UV spectra by an UV spectrophotometer with a diode array detector and their evaluation for identification purposes. Identification of an unknown drug.

10) Raman spectroscopy. Measurement and evaluation of Raman spectra for identification purposes. Identification of unknown drug.

11) Quantitative elemental analysis (EA), UV and IR spectrometry. Identification of an unknown organic compound with use of EA, UV and IR data.

12) Gas chromatography. Measurement and evaluation of chromatograms. GLC identification of organic compounds. Determination of pesticides permethrin and fenoxycarb in a veterinary preparation.

13) Polarimetric analysis. Quantitative polarimetric analysis of a sample containing unknown amount of glucose, sucrose or lactose.

14) High performance liquid chromatography (HPLC) I. Measurement and evaluation of chromatograms. Determination of sodium diclofenac in pharmaceutical preparations. ). Determination of hydrocortisone acetate in a test solution.

15) High performance liquid chromatography (HPLC) II. Optimization of the mobile phase for the UHPLC separation of a mixture of acidic, neutral and basic compounds.