Instrumental Methods - GAF301
Title: Instrumental Methods
Guaranteed by: Department of Analytical Chemistry (16-16140)
Faculty: Faculty of Pharmacy in Hradec Králové
Actual: from 2024
Semester: summer
Points: 0
E-Credits: 6
Examination process: summer s.:combined
Hours per week, examination: summer s.:14/56, C+Ex [HS]
Capacity: unlimited / unlimited (unknown)
Min. number of students: unlimited
4EU+: no
Virtual mobility / capacity: no
Key competences:  
State of the course: taught
Language: English
Teaching methods: full-time
Level:  
Note: deregister from the exam date if a requisite was not fulfilled
course can be enrolled in outside the study plan
enabled for web enrollment
Guarantor: doc. Burkhard Horstkotte, M.Sc., Dr.
Comes under: 2.ročník 2024/25 Pharmacy (EN19)
Co-requisite : GAF300
Interchangeability : GAF274
Is co-requisite for: GAF313, GAF302, GAF395, GAF314
Is pre-requisite for: GAF306, GAF385, GAF405
Examination dates   SS schedule   
Annotation -
The aim of the subject is to provide the students with firm and sufficiently wide theoretical and methodological fundamentals for pursuing (in a rational way) instrumental analysis of inorganic and organic substances. The teaching is focused on the explanation of theoretical aspects of instrumental methods and putting the accent on problem-solving tuition. In practical training individual approach of students to solving analytical problems is required.
Last update: Horstkotte Burkhard, doc., M.Sc., Dr. (02.08.2024)
Course completion requirements -

Requirements for credit and exam are based on:

Practical course

  1. Participation in all practical classes – (missing practical classes must be revisited or it can be substituted if permitted by the teacher)

  2. Submission of all reports of practical exercises

  3. Minimum 66% of points for correct results in practical tasks and for correct answers in the monitoring and credit tests

 

Exam

  1. The exam from Instrumental methods is organized in terms presented in the Study information system, the time of exam is always specified. Simple calculator is needed for written exam. Evaluation is carried out directly after evaluation of the test.

  2. The exam is organized together with the subject Analytical chemistry.

  3. For the exam, credits from both practical classes are needed.

  4. Exam organization:

The first term – written test + possibility of oral examination

The second term - written test + oral examination

The third term – oral examination

  1. Exam scope is specified in the Study materials – Study KACH – Instrumental methods

Last update: Horstkotte Burkhard, doc., M.Sc., Dr. (02.08.2024)
Literature -

Recommended:

  • . 1079. In Robinson, James W., Frame, Eileen M. Skelly Frame, George M.. Undergraduate instrumental analysis . New York: M. Dekker, 2005, s. -. ISBN 0-8247-5359-3..

Last update: prepocet_literatura.php (19.09.2024)
Syllabus -

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.

Last update: Horstkotte Burkhard, doc., M.Sc., Dr. (02.08.2024)
Learning outcomes

The Instrumental Methods course builds on the knowledge and skills acquired in the subjects: Physical Chemistry and Analytical Chemistry.

After completing the course, students will be able to use the following terms in the correct context towards the analytical evaluation of inorganic and organic substances using instrumental methods: spectrophotometry in the visible and UV region, potentiometry and its use for the evaluation of titration determinations, polarimetry for determining the content of optically active substances, identification of organic substances using optical techniques (IR and Raman spectrometry), use of melting point for identifying organic compounds, thin layer chromatography (design, detection, composition of stationary and mobile phases), high-performance liquid chromatography (normal and reverse phase, pH adjustment of the aqueous component of the mobile phase in reverse mode, detection), gas chromatography (capillary and packed columns, elution method, detection).

Learning outcomes:

Based on the acquired knowledge and skills, students will:

explain the procedure for determining an organic substance using spectrophotometry in the visible region, including derivatization, optimization of spectrophotometric determination, measurement of the calibration curve and its evaluation and applications for determining the content of a substance in the visible region of the spectrum;

explain the procedure for potentiometric indication of the equivalence point and various types of titration determinations, including the selection of an electrode system, evaluation of the titration curve and calculation of the content of the substance being determined;

define polarimetry as an instrumental method for assessing the purity/content of an optically active organic substance, including the procedure for measuring and calculating the content using specific optical rotation; explain the procedure for identifying an organic compound using various types of spectral methods, compare their approach and the information obtained, differences in the principle of these techniques, evaluate spectra and identify an organic compound;

explain the principle of identifying a compound by determining the melting point of this compound and its derivative;

explain the principle of thin-layer chromatography using silica gel as a stationary phase, describe the procedure, various methods of detection and evaluation of a chromatogram for identifying organic substances and their derivatives;

explain the principle of separation of analyte mixtures by HPLC, describe the system, characterize retention mechanisms, stationary and mobile phases in two basic chromatographic modes, describe detectors in HPLC and evaluation of chromatograms using an external or internal standard to identify and determine the content of organic substances in mixtures;

define for which substances GC is used for separation, explain the difference between LC and GC with regard to the stability of substances, temperature regime, and the principle of basic types of detectors.

Last update: Horstkotte Burkhard, doc., M.Sc., Dr. (25.02.2025)