Analytical NMR

Cairo university

Faculty of pharmacy

Analytical chemistry

department

NMR Spectroscopy

Explaining NMR

UV/Vis spectroscopy

Sample

Nuclear magnetic resonance

spectroscopy

• Def. :-known as NMR spectroscopy, is a research technique that exploits the magnetic properties of certain a certain atomic nuclei.

• . It determines the physical and chemical properties of atoms in which they are contained.

•Basic NMR techniques:-

1-The NMR sample is prepared in a thin-walled glass tube - a NMR tube.

2-When placed in a magnetic field, NMR active nuclei (such as 1H or 13C) absorb electromagnetic radiation .

• Now we have to answer an important question, on which phenomenon it relies ?

• As an answer for this question we will ay it depends on nuclear magnetic resonance.

• Importance :-1-Can provide detailed information about the

structure, dynamics, reaction state, and chemical environment of molecules.

2-is used by chemists and biochemists to investigate the properties of organic molecules at a frequency characteristic of the isotope.

•Now it is time to talk about the chemical shift.

• What is chemical shift?

•Chemical shift:-is the resonant frequency of a nucleus relative to a standard, this standard is often tetramethylsilane, Si(CH3)4, abbreviated TMS.

Example of the chemical shift:• NMR spectrum of hexaborane

B6H10 showing peaks shifted in frequency, which give clues as to the molecular structure.

• Importance :-The chemical shift provides information about the structure of the molecule.

• Do you remember spin-spin coupling?

• It a special type of it. This coupling arises

from the interaction of different spin states

through the chemical bonds of a molecule

and results in the splitting of NMR signals.

• Importance:-it provides detailed insight

into the connectivity of atoms in a

molecule.

NMR analysis applications

1-Chemical structure analysis of liquids and dissolved solids

2-Deformulation of products

3-Quantification of mixture components

NMR analysis capabilities :

1- Quantitative NMR Analysis (qNMR)

solid State Nuclear Magnetic Resonance-23-Solution State NMR

4-NMR Chemical Composition

5-Elucidation

NMR analysis expertise.

laboratories provide clients analytical data regarding the type, quantity and arrangement of atoms in chemical systems, liquids and solids.

1-Quantitative NMR Analysis :-

Intertie NMR laboratories provide qNMR (Quantitative Nuclear Magnetic Resonance Spectroscopy) analysis applications such as quality control, drug impurity analysis, and metabonomicsin agrochemicals, chemicals, plastics processing and the pharmaceutical industry

2-Solid State Nuclear Magnetic Resonance

Solid state Nuclear Magnetic Resonance (NMR) is a specialized characterization technique used to determine chemical composition or structural properties in a variety of industrially relevant materials. Solid State NMR brings the benefits of solutions NMR (detailed chemical structural information without the need for standards

Heterogeneous catalysts used for chemical manufacture, petroleum processes, purification, and air separationDetermine framework composition of zeolites and changes with activation or useIdentify adsorbed species in porous materialsCharacterize key functionalities in insoluble residues

Determination of catalyst

• Correlation spectroscopy:-

•is one of several types of two-dimensional nuclear magnetic resonance (NMR) spectroscopy .This type of NMR experiment is best known by its acronym .

• Biomolecular NMR spectroscopy:-• A-proteins:-Much of the innovation within

NMR spectroscopy has been within the field of protein NMR spectroscopy, an important technique in structural biology .

• B-Nuculeic acids :-

• is the use of NMR spectroscopy to obtain information about the structure and dynamics of polynuculeic acid, such as DNA or RNA.

• Note :-Nucleic acid and protein NMR spectroscopy are similar but differences exist. Nucleic acids have a smaller percentage of hydrogen atoms, which are the atoms usually observed in NMR spectroscopy.

1937 Rabi predicts and observes nuclear magnetic

resonance

1946 Bloch, Purcell first nuclear magnetic resonance of

bulk sample

1966 Ernst, Anderson Fourier transform NMR

1944 Physics Rabi (Columbia)

1952 Physics Bloch (Stanford), Purcell (Harvard)

1991 Chemistry Ernst (ETH)

2003 Medicine Lauterbur (University of Illinois in Urbana)

NMR History

Some NMR Web Sites

The Basics of NMR by J.P. Hornak Hypertext based NMR course http://www.cis.rit.edu/htbooks/nmr/nmr-main.htm

Integrated Spectral Data Base System for Organic Compoundshttp://www.aist.go.jp/RIODB/SDBS/menu-e.html

Educational NMR Software All kinds of NMR softwarehttp://www.york.ac.uk/depts/chem/services/nmr/edusoft.html

NMR Knowledge Base A lot of useful NMR linkshttp://www.spectroscopynow.com/

NMR Information Server News, Links, Conferences, Jobshttp://www.spincore.com/nmrinfo/

Technical Tidbits Useful source for the art of shimminghttp://www.acornnmr.com/nmr_topics.htm

BMRB (BioMagResBank) Database of NMR resonance assignmentshttp://www.bmrb.wisc.edu/

To

Our doctors

Dr /ghada moustafa

Dr /esraa fawaaz

DutiesNumbersNames

Data Collector20452Sally Yousry

Data Collector + summarizer + powerpoint

+ leader

20453Sameh Gamal

presenter20455Sandra Maher

Data Collector20456Sandy Maged

Data Collector20457Sahar Ezzat

Data Collector20458Sahar Mahmoud

Data Collector + powerpoint + presenter20459Salma Ahmed

Data Collector + summarizer20460Salma Gamal