SubjectsSubjects(version: 945)
Course, academic year 2023/2024
   Login via CAS
NMP Spectroscopy of condensed state - MC260P125
Title: NMR spektroskopie kondenzovaného stavu
Czech title: NMR spektroskopie kondenzovaného stavu
Guaranteed by: Department of Physical and Macromolecular Chemistry (31-260)
Faculty: Faculty of Science
Actual: from 2022
Semester: winter
E-Credits: 3
Examination process: winter s.:
Hours per week, examination: winter s.:2/0, Ex [HT]
Capacity: unlimited
Min. number of students: unlimited
4EU+: no
Virtual mobility / capacity: no
State of the course: taught
Language: Czech, English
Note: enabled for web enrollment
Guarantor: Ing. Jiří Brus, Dr.
Teacher(s): Ing. Jiří Brus, Dr.
Annotation -
Last update: Ing. Jiří Brus, Dr. (09.02.2022)
This course introduces to students not only the basic principles of solid-state NMR spectroscopy, but also presents the current trends that allow for a detailed analysis of the structure and dynamics of condensed matter. The course is focused on the application of advanced NMR spectroscopy techniques for assessing the structure and dynamics of various multi-component nanostructured systems with hierarchically defined architecture. The basic principles of these techniques are discussed in the introductory parts of the lectures. Experimental procedures are then always demonstrated on typical examples, with the greatest attention being paid to interpretations of experimental data. Step-by-step, polymer composites and nanocomposites, pharmaceutical systems, polymeric nanoparticles and microparticles, liquid-crystalline and liquisolid systems, organogels and framework materials are investigated, spectroscopically decomposed on individual components and their structures thoroughly discussed. Considerable attention is paid to both collective processes and structural defects and the possibilities of their identification. Courses is held in English or Czech.
Literature - Czech
Last update: Ing. Jiří Brus, Dr. (23.05.2022)

·         Andrew E. Derome – Modern NMR Techniques for Chemistry Research, Pergamon Press (1987).

·         Melinda J. Duer – Introduction to Solid-state NMR Spectroscopy, Blackwell Publishing (2004).

·         K. Schmidt-Rohr, H.W. Spiess – Multidimensional Solid-state NMR and Polymers, Academic Press (1994).

·         K.J.D. Mackenzie, M.E. Smith – Multinuclear Solid-state NMR of Inorganic Materials, Pergamon (2002).

Requirements to the exam - Czech
Last update: Ing. Jiří Brus, Dr. (09.02.2022)

Zkouška bude probíhat písemnou formou v podobě testu, který je tematicky rozdělen do 10 okruhů. Tyto okruhy přímo sledují témata jednotlivých přednášek. Test je možno vyplnit v českém i anglickém jazyce podle preference studenta. Požadovanou formou zpracování otázek jsou krátké úvahy, případně komentáře doplněné grafy nebo schématy. Minimální rozsah celé práce jsou cca 3-4 strany A4.

Test bude zadán po poslední přednášce (zaslán e-mailem v elektronické podobě). Ke zpracování úkolu lze použít veškerou dostupnou literaturu, včetně podkladů k přednáškám. Přednášející nabízí možnost konzultací on-line formou. Datum odevzdání vyplněného testu je obvykle konec semestru (zkouškového období) a bude vždy přesně specifikován. Zpracovaný test se bude odesílat e-mailem v elektronické podobě na brus@imc.cas.cz. Hodnocení zpracovaného testu proběhne během následujícího týdne.

The exam will be written in the form of a test divided into 10 topics. These sections directly follow the topics of the individual lectures. The test can be completed in Czech or English according to the student's preference. The required form of answers are short reflections or comments accompanied by graphs or diagrams. The minimum size of the completed test is about three-four A4 pages.

The test will be given after the last lecture (sent by an e-mail in the electronic form). All available literature, including lecture handouts, may be used for the assignment. The lecturer offers the possibility of on-line consultation. The due date for the completed test is usually the end of the semester (the exam period) and will always be specified. The completed test will be emailed electronically to brus@imc.cas.cz. Assessment of the completed test will take place during the following week.

 

 

Syllabus -
Last update: Ing. Jiří Brus, Dr. (09.02.2022)

1. Basic principles of ss-NMR spectroscopy and historical overview

The first lecture is devoted to the basic principles of ss-NMR spectroscopy. These principles are discussed in the context of historical milestones.

2. Architecture of liquisolid systems and invisible (dark) matter in ss-NMR

The second lecture is focused on a very interesting aspect of liquisolid systems, their structure, architecture, formation of exotic phases. In this regard the basic experimental techniques, their selectivity and limitations will be again discussed. This is also perfect occasion to open the discussion of the invisible matter in solid state.

3. Structural diversity of solid dispersions: structure, morphology and phase-transitions

In the third lecture the structural diversity of solid dispersions and other multicomponent solids is discussed.

4. Polymorphism of pharmaceutical solids: NMR crystallography

Polymorphism of pharmaceutical solids, crystalline active pharmaceutical ingredients and introduction to NMR crystallography is the topic of the fourth lecture.

5. Crystal structure predictions and domain-edited NMR crystallography

In the fifth lecture we will continue with the discussion of NMR crystallography. Specifically, we will talk about the crystal structure prediction, their experimental verification, and application of NMR crystallography on multicomponent and polycrystalline mixtures.

6. A story about an unknown structure of a well-known ss-NMR model compound

The true potential of NMR crystallography in the ab-initio, de-nuovo, determination of crystal structure will be demonstrated on an f-MLF tripeptide, whose structure has not yet been determined. You will be among the first to see it.

7. What about quadrupolar nuclei? Structural diversity of boronic acid derivatives.

In the subsequent lecture we will turn our attention to quadrupolar nuclei, specifically, to boron-11. In this regard we will discuss dynamic self-assemble processes of derivatives of boronic acid.

8. Amorphous solids and principal component analysis

Amorphous phase. The structure of amorphous phase is a bit mysterious. One of the possible insights into the structure of amorphous phase can be obtained through the principal component analysis of NMR spectra. And particularly this analysis is a subject of the eighth lecture.

9. Conductivity and transferring Li+ ions in solid state

Going gradually to the end of the course we will open the question of the dynamics, transfer and local mobility of Li ions in polymer matrices and framework materials – potential all-solid-state electrolytes.

10. Frameworks, networks and crosslinks

One of the last lectures will be devoted to the structure of metal-organic frameworks, polymer networks and their cross-links.

11. Summary: challenges, potentials and limitations of ss-NMR

The last lecture will summarize all the previous presentations and show potentialities, limitations and challenges of advanced solid-state NMR spectroscopy.

 
Charles University | Information system of Charles University | http://www.cuni.cz/UKEN-329.html