Double-Resonance Experiments
|
|
- Lindsay Turner
- 5 years ago
- Views:
Transcription
1 Double-Resonance Eperiments The aim - to simplify complicated spectra by eliminating J-couplings. omonuclear Decoupling A double resonance eperiment is carried out using a second rf source B 2 in addition to the rf transmitter B 1 used for the detection of the spectrum. omonuclear spin pair AX with a scalar J AX 0: if we observe the A nucleus while irradiating selectively the X nucleus, the scalar coupling J AX vanishes. The necessary strength of the B 2 field: γb 2 /2π > 2J AX. In terms of the vector model: the frequency ν 2 = γb 2 /2π coincides with the Larmor frequency of the X nucleus B eff = B 2, i.e., the vector µ X precesses around B 2 and thus around ais. The nuclear spin vectors I A and I X are then quantized along the z- and the -ais respectively. They are orthogonal and their scalar product (E = J AX I A I X ) is therefore zero (the scalar spin-spin coupling vanishes). For simple spectra, the results are straightforward: record two spectra, one with and another without selective decoupling and check which multiplets change. For more crowded spectra, it is common to take the difference between the two spectr a in order to observe changes that would otherwise be difficult to detect. O B2 O O N O ppm ppm ppm NMR Spectroscopy 1
2 Main problems: (i) suffers from difficulties associated with selective irradiatiation of only those spins which are desired; (ii) Bloch-Siegert shift: ν ' A γ B ν A + 8π 2 ( ν ν ) A 2 2 X If several spin-decoupling eperiments are desired, it is generally more time-efficient to perform a twodimensional COSY eperiment in order to establish connectivities. eteronuclear Decoupling The frequency difference ν 2 - ν 1 lies in the Mz range. The second field B 2 is produced by a separate transmitter. 1{ 14 N} NMR N 4 + A curly bracket is used to indicate which nucleus is being decoupled during the eperiment, e.g. 13C{1} indicates a 13C spectrum acquired with 1 decoupling. Can be used for simplifying spectra complicated by heteronuclear J-couplings (e.g., J F or J P ) or for removing line broadening caused by quadrupolar nuclei (e.g., 14 N). 1 NMR N 4 + Broadband decoupling Broadband decoupling is used in order to eliminate the coupling between two nuclei completely. For eample, broadband 1 decoupling while acquiring 13 C spectrum leads to singlets for each 13 C environment and a substantial increase in the sensitivity of the eperiment. Previously broadband decoupling techniques were based on the combined use of high-power decoupling and frequency modulation of the B 2 frequency with a randomly varying waveform (proton noise decoupling). Generally, this results in an inefficient broadband decoupling and leads to loss of both sensitivity and resolution. Broadband decoupling techniques based upon the spin flip eperiment (MLEV, Malcolm Levitt): 1 π τ π τ π τ π τ π τ C π/2 Acquire... NMR Spectroscopy 2
3 180 ( 1 ) -J/2 +J/2 +J/2 -J/2 On Off τ 2τ ADC A train of π pulses will be susceptible to the errors due to pulse length inaccuracy, since they will accumulate. The non-ideal π pulse can be replaced with a composite pulse. Composite π y pulse: π π y Eamples of composite pulse decoupling techniques: WALTZ-16 and GARP The linewidth achievable in WALTZ C NMR spectra is ~ z (suitable for detecting small effects such as 35/37 Cl isotope effects of a few ppb) conventional modulation technique; composite pulse decoupling kz Broadband decoupling of nuclei with large chemical shift ranges ( 19 F, 31 P) with 1 observation becomes much more feasible on using such decoupling techniques as GARP. The effective decoupling bandwidth: WALTZ-16 Gated decoupling GARP-1 2B 2 (B 2 5 kz) 5B 2 (slightly greater residual broadening of the lines) Disadvantages of 13 C{ 1 } spectra: (i) the nuclear Overhauser effect (NOE) leads to intensity distortions and the integration of these spectra becomes questionable; (ii) the elimination of line splittings prevents the measurement of 13 C, 1 coupling constants. NMR Spectroscopy 3
4 The application of a method known as gated decoupling eperiment successfully handles spin-spin coupling and intensity distortions. In the first case, the decoupler is switched on during acquisition, but switched off during the remaining time before the net pulse. The 13 C- 1 coupling is thus eliminated without producing NOE, as the integrals depend mainly on the intensities of the initial points of the time domain function. B 1 NOE Alternatively, relaation reagents (e.g., chromium acetylacetonate) can be used to eliminate unwanted NOEs. Because of their paramagnetic moment, relaation reagents provide an efficient mechanism for 13 C spin-lattice relaation that suppresses dipolar relaation, which is the main phenomenon leading to NOEs. B 2 In the second case, the decoupler is gated: it is on during the delay time between different pulses and switched off during acquisition. FID FID B 1 NOE B 2 As a result, the spectra are not decoupled and most of the NOE is preserved. This provides higher sensitivity for measurements of J( 13 C, 1 ) couplings. NMR Spectroscopy 4
5 Eample of signal multiplicities in a proton-coupled 13 C NMR spectrum 13 C, 1 coupling constants in pyridine C-3 2 J(4) 2 z 3 J(5) 6 z 2J(2) 7 z 1J(3) 166 z C-4 C-3 C ppm 3J(2) 4 z 1 J(4) 163 z ppm N C-2 2 J(3) 2 z 3J(4) 7 z 3J(6) 12 z 1 J(2) 177 z C ppm NMR Spectroscopy 5
6 Polarization Transfer The aim - to increase sensitivity by transferring favourable NMR properties of the proton to another nucleus. N β / N α = ep (- E / kt) 1 - E / kt = 1 - γh B 0 / kt n = N α N β n γh B 0 / kt Selective population inversion A two-spin system 1-13 C (e.g., in CCl 3 ) h c C 2 h+ c 1 {INVERTED} - h+ c C 2 - h- c 1 2 h+ c C 1 h c 2 h- c h+ c C C 1 13C γ 4 γ C h 4 c C +1 : +1 3 : +5 Relative intensities for the X multiplet of an AX n group: at Boltzmann distribution after selective population inversion n NMR Spectroscopy 6
7 INEPT (Insensitive Nuclei Enhanced by Polarization Transfer) 1 : π τ π τ 2 13 C: π τ = 1 / (4 1 J C ) y Acquire Non-selective pulses are used to put pairs of proton transitions into antiphase /(4J) 180 1/(4J) 90 y The proton magnrtisation vectors are prepared in antiphase: the α vector along +z and the β vector along -z (as in SPI). This corresponds to inverted 1 spin populations with the ecess population in the upper level. A 1 13 C polarization transfer occurs and a fourfold (γ /γ C ) enhancement in 13 C signal-to-noise ratio is achieved. As relaation times T 1 ( 1 ) are shorter than T 1 ( 13 C), there is a further gain in the rate at which signals can be accumulated. DEPT (Distortionless Enhancement by Polarization Transfer) J 2J ± y 2J 1 : π θ ( Decouple ) 13 C: π ± Acquire( ) θ ±y a pulse of variable length. To separate C, C 2 and C 3 subspectra, eperiments with θ = π/4, π/2 and 3π/4 are performed. NMR Spectroscopy 7
τ 1 > 1/J - if this lifetime is significantly shortened, the coupling (splitting of the signal) will not be observed
It is often advantageous to reverse or remove the splitting caused by spin-spin coupling This is called spin decoupling Spin decoupling (or just decoupling) can be used for several reasons - to simplify
More informationNMR Spectroscopy: A Quantum Phenomena
NMR Spectroscopy: A Quantum Phenomena Pascale Legault Département de Biochimie Université de Montréal Outline 1) Energy Diagrams and Vector Diagrams 2) Simple 1D Spectra 3) Beyond Simple 1D Spectra 4)
More informationNMR course at the FMP: NMR of organic compounds and small biomolecules - II -
NMR course at the FMP: NMR of organic compounds and small biomolecules - II - 16.03.2009 The program 2/76 CW vs. FT NMR What is a pulse? Vectormodel Water-flip-back 3/76 CW vs. FT CW vs. FT 4/76 Two methods
More informationONE AND TWO DIMENSIONAL NMR SPECTROSCOPY
ONE AND TWO DIMENSIONAL NMR SPECTROSCOPY Atta-ur-Rahman H.E.J. Research Institute of Chemistry, University ofkarachi, Karachi 32, Pakistan ELSEVIER Amsterdam Oxford New York Tokyo 1989 IX CONTENTS Chapter-l
More informationChemistry 431. Lecture 23
Chemistry 431 Lecture 23 Introduction The Larmor Frequency The Bloch Equations Measuring T 1 : Inversion Recovery Measuring T 2 : the Spin Echo NC State University NMR spectroscopy The Nuclear Magnetic
More informationIntroduction to 1D and 2D NMR Spectroscopy (4) Vector Model and Relaxations
Introduction to 1D and 2D NMR Spectroscopy (4) Vector Model and Relaxations Lecturer: Weiguo Hu 7-1428 weiguoh@polysci.umass.edu October 2009 1 Approximate Description 1: Energy level model Magnetic field
More informationCarbon 13 NMR NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY
NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY PRINCIPLE AND APPLICATION IN STRUCTURE ELUCIDATION Carbon 13 NMR Professor S. SANKARARAMAN Department of Chemistry Indian Institute of Technology Madras Chennai
More informationC NMR Spectroscopy
13.14 13 C NMR Spectroscopy 1 H and 13 C NMR compared: both give us information about the number of chemically nonequivalent nuclei (nonequivalent hydrogens or nonequivalent carbons) both give us information
More informationMagnetic Resonance Spectroscopy
INTRODUCTION TO Magnetic Resonance Spectroscopy ESR, NMR, NQR D. N. SATHYANARAYANA Formerly, Chairman Department of Inorganic and Physical Chemistry Indian Institute of Science, Bangalore % I.K. International
More informationThe NMR Spectrum - 13 C. NMR Spectroscopy. Spin-Spin Coupling 13 C NMR. A comparison of two 13 C NMR Spectra. H Coupled (undecoupled) H Decoupled
Spin-Spin oupling 13 NMR A comparison of two 13 NMR Spectra 1 oupled (undecoupled) 1 Decoupled 1 Proton Decoupled 13 NMR 6. To simplify the 13 spectrum, and to increase the intensity of the observed signals,
More information8.2 The Nuclear Overhauser Effect
8.2 The Nuclear Overhauser Effect Copyright Hans J. Reich 2016 All Rights Reserved University of Wisconsin An important consequence of DD relaxation is the Nuclear Overhauser Effect, which can be used
More informationTwo Dimensional (2D) NMR Spectroscopy
The two important parameters obtained from NMR spectra are; Two Dimensional (2D) NMR Spectroscopy py Correlation NMR a. Chemical shift b. Spin-spin coupling constant Large molecules with numerous atoms
More informationSpin Dynamics Basics of Nuclear Magnetic Resonance. Malcolm H. Levitt
Spin Dynamics Basics of Nuclear Magnetic Resonance Second edition Malcolm H. Levitt The University of Southampton, UK John Wiley &. Sons, Ltd Preface xxi Preface to the First Edition xxiii Introduction
More informationCHEM / BCMB 4190/6190/8189. Introductory NMR. Lecture 10
CHEM / BCMB 490/690/889 Introductory NMR Lecture 0 - - CHEM 490/690 Spin-Echo The spin-echo pulse sequence: 90 - τ - 80 - τ(echo) Spins echoes are widely used as part of larger pulse sequence to refocus
More informationConcepts on protein triple resonance experiments
2005 NMR User Training Course National Program for Genomic Medicine igh-field NMR Core Facility, The Genomic Research Center, Academia Sinica 03/30/2005 Course andout Concepts on protein triple resonance
More informationNuclear Magnetic Resonance Spectroscopy
Nuclear Magnetic Resonance Spectroscopy Structural Elucidation Nuclear magnetic resonance spectroscopy is the name given to the technique which exploits the magnetic properties of nuclei and measures their
More informationPolarization transfer
Polarization transfer So far we have dealt vectors (magnetizations) that are proportional to the sensitivit of the nuclei we are studing. In multiple pulse eperiments, were we are doing man things to a
More informationChem 325 NMR Intro. The Electromagnetic Spectrum. Physical properties, chemical properties, formulas Shedding real light on molecular structure:
Physical properties, chemical properties, formulas Shedding real light on molecular structure: Wavelength Frequency ν Wavelength λ Frequency ν Velocity c = 2.998 10 8 m s -1 The Electromagnetic Spectrum
More informationSpin-spin coupling I Ravinder Reddy
Spin-spin coupling I Ravinder Reddy Spin-interactions External interactions Magnetic field Bo, RF field B1 Internal Interactions Molecular motions Exchange Chemical shifts J-coupling Spin Diffusion Dipolar
More informationPROTEIN NMR SPECTROSCOPY
List of Figures List of Tables xvii xxvi 1. NMR SPECTROSCOPY 1 1.1 Introduction to NMR Spectroscopy 2 1.2 One Dimensional NMR Spectroscopy 3 1.2.1 Classical Description of NMR Spectroscopy 3 1.2.2 Nuclear
More information10.4 Continuous Wave NMR Instrumentation
10.4 Continuous Wave NMR Instrumentation coherent detection bulk magnetization the rotating frame, and effective magnetic field generating a rotating frame, and precession in the laboratory frame spin-lattice
More information4 DQF-COSY, Relayed-COSY, TOCSY Gerd Gemmecker, 1999
44 4 DQF-COSY, Relayed-COSY, TOCSY Gerd Gemmecker, 1999 Double-quantum filtered COSY The phase problem of normal COSY can be circumvented by the DQF-COSY, using the MQC term generated by the second 90
More informationThe NMR Inverse Imaging Problem
The NMR Inverse Imaging Problem Nuclear Magnetic Resonance Protons and Neutrons have intrinsic angular momentum Atoms with an odd number of proton and/or odd number of neutrons have a net magnetic moment=>
More informationPrincipios Básicos de RMN en sólidos destinado a usuarios. Gustavo Monti. Fa.M.A.F. Universidad Nacional de Córdoba Argentina
Principios Básicos de RMN en sólidos destinado a usuarios Gustavo Monti Fa.M.A.F. Universidad Nacional de Córdoba Argentina CONTENIDOS MODULO 2: Alta resolución en sólidos para espines 1/2 Introducción
More informationNMR, the vector model and the relaxation
NMR, the vector model and the relaxation Reading/Books: One and two dimensional NMR spectroscopy, VCH, Friebolin Spin Dynamics, Basics of NMR, Wiley, Levitt Molecular Quantum Mechanics, Oxford Univ. Press,
More informationCOSY type experiments exploring through-bond homonuclear correlations
COSY type experiments exploring through-bond homonuclear correlations Assistant Professor Kenneth Kongstad Bioanalytical Chemistry and Metabolomics Research Group Section for Natural Products and Peptides
More informationChapter 7. Nuclear Magnetic Resonance Spectroscopy
Chapter 7 Nuclear Magnetic Resonance Spectroscopy I. Introduction 1924, W. Pauli proposed that certain atomic nuclei have spin and magnetic moment and exposure to magnetic field would lead to energy level
More informationInverse Detection in Multinuclear NMR
Inverse Detection in Multinuclear NMR The HETCOR experiment is an example of a directly-detected heteronuclear experiment. The timing diagram for the most basic form of the HETCOR pulse sequence is shown
More informationTopics. Spin. The concept of spin Precession of magnetic spin Relaxation Bloch Equation
Bioengineering 280A Principles of Biomedical Imaging Fall Quarter 2005 MRI Lecture 1 Topics The concept of spin Precession of magnetic spin Relaation Bloch Equation Spin Intrinsic angular momentum of elementary
More informationInterferogram and real-time acquisition methods
Interferogram and real-time acquisition methods Peter Kiraly NMR Methodology Group, School of Chemistry, University of Manchester Workshop on Pure Shift NMR 2 th Sep 207 Outline Why are we interested in
More informationFinal Exam: CHEM/BCMB 4190/6190/8189 (276 pts) Thursday, 15 December, 2005
Final Eam: CHEM/BCMB 4190/6190/8189 (276 pts) Thursda, 15 December, 2005 1). The two-proton spin sstem at right gives rise to the 1 H NMR spectra shown (spectra 1 and 2, below) as the ratio of /J changes
More informationRelaxation, Multi pulse Experiments and 2D NMR
Relaxation, Multi pulse Experiments and 2D NMR To Do s Read Chapter 6 Complete the end of chapter problems; 6 1, 6 2, 6 3, 6 5, 6 9 and 6 10. Read Chapter 15 and do as many problems as you can. Relaxation
More informationClassical behavior of magnetic dipole vector. P. J. Grandinetti
Classical behavior of magnetic dipole vector Z μ Y X Z μ Y X Quantum behavior of magnetic dipole vector Random sample of spin 1/2 nuclei measure μ z μ z = + γ h/2 group μ z = γ h/2 group Quantum behavior
More informationMagnetic Nuclei other than 1 H
Magnetic Nuclei other than 1 H 2 H (Deuterium): I = 1 H,D-Exchange might be used to simplify 1 H-NMR spectra since H-D couplings are generally small; - - - -O- - - -D 2 -O- triplet of triplets slightly
More informationSpectral Broadening Mechanisms
Spectral Broadening Mechanisms Lorentzian broadening (Homogeneous) Gaussian broadening (Inhomogeneous, Inertial) Doppler broadening (special case for gas phase) The Fourier Transform NC State University
More informationPrinciples of Nuclear Magnetic Resonance in One and Two Dimensions
Principles of Nuclear Magnetic Resonance in One and Two Dimensions Richard R. Ernst, Geoffrey Bodenhausen, and Alexander Wokaun Laboratorium für Physikalische Chemie Eidgenössische Technische Hochschule
More information4. Basic Segments of Pulse Sequences
4. Basic egments of Pulse equences The first applications of 2D NMR for studies of proteins in aqueous solution used only very few pulse sequences [5 7]. Today, a vast number of experimental schemes exist
More informationNMR Nuclear Magnetic Resonance Spectroscopy p. 83. a hydrogen nucleus (a proton) has a charge, spread over the surface
NMR Nuclear Magnetic Resonance Spectroscopy p. 83 a hydrogen nucleus (a proton) has a charge, spread over the surface a spinning charge produces a magnetic moment (a vector = direction + magnitude) along
More informationHigh-Resolutio n NMR Techniques i n Organic Chemistry TIMOTHY D W CLARIDGE
High-Resolutio n NMR Techniques i n Organic Chemistry TIMOTHY D W CLARIDGE Foreword Preface Acknowledgements V VI I X Chapter 1. Introduction 1.1. The development of high-resolution NMR 1 1.2. Modern
More informationNMR: PRACTICAL ASPECTS
NMR: PRACTICAL ASPECTS Pedro M. Aguiar Sample Preparation Well prepared sample can yield high quality spectra Poorly prepared sample typically yields low quality spectra Tubes of appropriate quality Higher
More informationThe Use of NMR Spectroscopy
Spektroskopi Molekul Organik (SMO): Nuclear Magnetic Resonance (NMR) Spectroscopy All is adopted from McMurry s Organic Chemistry The Use of NMR Spectroscopy Used to determine relative location of atoms
More informationGeneral NMR basics. Solid State NMR workshop 2011: An introduction to Solid State NMR spectroscopy. # nuclei
: An introduction to Solid State NMR spectroscopy Dr. Susanne Causemann (Solid State NMR specialist/ researcher) Interaction between nuclear spins and applied magnetic fields B 0 application of a static
More informationCHEM 322 Laboratory Methods in Organic Chemistry. Introduction to NMR Spectroscopy
EM 322 Laboratory Methods in Organic hemistry Introduction to NMR Spectroscopy What structural information does NMR spectroscopy provide? 1) hemical shift (δ) data reveals the molecular (functional group)
More informationBasic One- and Two-Dimensional NMR Spectroscopy
Horst Friebolin Basic One- and Two-Dimensional NMR Spectroscopy Third Revised Edition Translated by Jack K. Becconsall WILEY-VCH Weinheim New York Chichester Brisbane Singapore Toronto Contents XV 1 The
More informationBiochemistry 530 NMR Theory and Practice
Biochemistry 530 NMR Theory and Practice David Baker Autumn Quarter 2014 Slides Courtesy of Gabriele Varani Recommended NMR Textbooks Derome, A. E. (1987) Modern NMR Techniques for Chemistry Research,
More informationNuclear Magnetic Resonance Spectroscopy
Nuclear Magnetic Resonance Spectroscopy Ecole Polytechnique Département de Chimie CHI 551 Dr. Grégory Nocton Bureau 01 30 11 A Tel: 44 02 Ecole polytechnique / CNRS Laboratoire de Chimie Moléculaire E-mail:
More informationWith that first concept in mind, it is seen that a spinning nucleus creates a magnetic field, like a bar magnet
NMR SPECTROSCOPY This section will discuss the basics of NMR (nuclear magnetic resonance) spectroscopy. Most of the section will discuss mainly 1H or proton spectroscopy but the most popular nuclei in
More informationBiophysical Chemistry: NMR Spectroscopy
Relaxation & Multidimensional Spectrocopy Vrije Universiteit Brussel 9th December 2011 Outline 1 Relaxation 2 Principles 3 Outline 1 Relaxation 2 Principles 3 Establishment of Thermal Equilibrium As previously
More informationIntroduction to Relaxation Theory James Keeler
EUROMAR Zürich, 24 Introduction to Relaxation Theory James Keeler University of Cambridge Department of Chemistry What is relaxation? Why might it be interesting? relaxation is the process which drives
More informationIntroduction of Key Concepts of Nuclear Magnetic Resonance
I have not yet lost that sense of wonder, and delight, that this delicate motion should reside in all ordinary things around us, revealing itself only to those who looks for it. E. M. Purcell, Nobel Lecture.
More informationPAPER No. 12: ORGANIC SPECTROSCOPY. Module 19: NMR Spectroscopy of N, P and F-atoms
Subject Chemistry Paper No and Title Module No and Title Module Tag Paper 12: Organic Spectroscopy CHE_P12_M19_e-Text TABLE OF CONTENTS 1. Learning Outcomes 2. 15 N NMR spectroscopy 3. 19 F NMR spectroscopy
More informationMeasuring Spin-Lattice Relaxation Time
WJP, PHY381 (2009) Wabash Journal of Physics v4.0, p.1 Measuring Spin-Lattice Relaxation Time L.W. Lupinski, R. Paudel, and M.J. Madsen Department of Physics, Wabash College, Crawfordsville, IN 47933 (Dated:
More informationSSSC Discovery Series NMR2 Multidimensional NMR Spectroscopy
SSSC Discovery Series NMR2 Multidimensional NMR Spectroscopy Topics: 1. Some Common Experiments 2. Anatomy of a 2D experiment 3. 3D NMR spectroscopy no quantum mechanics! Some Common 2D Experiments Very
More informationMR Fundamentals. 26 October Mitglied der Helmholtz-Gemeinschaft
MR Fundamentals 26 October 2010 Mitglied der Helmholtz-Gemeinschaft Mitglied der Helmholtz-Gemeinschaft Nuclear Spin Nuclear Spin Nuclear magnetic resonance is observed in atoms with odd number of protons
More informationNMR NEWS June To find tutorials, links and more, visit our website
Department of Chemistry NMR Facilities Director: Dr. Carlos A. Steren NMR NEWS June 2014 To find tutorials, links and more, visit our website www.chem.utk.edu/facilities/nmr Computers and software updates
More information[1] [2] 10 CH 3 COOH 9 1D 1 H NMR
1.00 0.97 1.03 2.08 1.25 1.08 3.02 rganic NMR quick guide 2016 TDWC NMR Techniques in rganic Chemistry: a quick guide The NMR spectrum proves to be of great utility in structure elucidation because the
More informationMagnetisation Transfer Schemes
Magnetisation Transfer Schemes P. K. Madhu Department of Chemical Sciences Tata Institute of Fundamental Research Homi Bhabha Road Colaba Mumbai 400 005, India Sensitivity of NMR Spectroscopy S/N Nγ exc
More information4 Spin-echo, Spin-echo Double Resonance (SEDOR) and Rotational-echo Double Resonance (REDOR) applied on polymer blends
4 Spin-echo, Spin-echo ouble Resonance (SEOR and Rotational-echo ouble Resonance (REOR applied on polymer blends The next logical step after analyzing and concluding upon the results of proton transversal
More information5 Heteronuclear Correlation Spectroscopy
61 5 Heteronuclear Correlation Spectroscopy H,C-COSY We will generally discuss heteronuclear correlation spectroscopy for X = 13 C (in natural abundance!), since this is by far the most widely used application.
More information1. 3-hour Open book exam. No discussion among yourselves.
Lecture 13 Review 1. 3-hour Open book exam. No discussion among yourselves. 2. Simple calculations. 3. Terminologies. 4. Decriptive questions. 5. Analyze a pulse program using density matrix approach (omonuclear
More informationSolid-state NMR and proteins : basic concepts (a pictorial introduction) Barth van Rossum,
Solid-state NMR and proteins : basic concepts (a pictorial introduction) Barth van Rossum, 16.02.2009 Solid-state and solution NMR spectroscopy have many things in common Several concepts have been/will
More informationCenter for Sustainable Environmental Technologies, Iowa State University
NMR Characterization of Biochars By Catherine Brewer Center for Sustainable Environmental Technologies, Iowa State University Introduction Nuclear magnetic resonance spectroscopy (NMR) uses a very strong
More informationPolarised Nucleon Targets for Europe, 2nd meeting, Bochum 2005
Polarised Nucleon Targets for Europe, nd meeting, Bochum Temperature dependence of nuclear spin-lattice relaxations in liquid ethanol with dissolved TEMPO radicals H. Štěpánková, J. Englich, J. Kohout,
More informationIndirect Coupling. aka: J-coupling, indirect spin-spin coupling, indirect dipole-dipole coupling, mutual coupling, scalar coupling (liquids only)
Indirect Coupling aka: J-coupling, indirect spin-spin coupling, indirect dipole-dipole coupling, mutual coupling, scalar coupling (liquids only) First, two comments about direct coupling Nuclear spins
More informationMultidimensional NMR Experiments
Multidimensional NMR Experiments Chem 8361/4361: Interpretation of rganic Spectra 2009 2013 Andrew arned & Regents of the University of Minnesota General Information More complicated experiments to set
More informationX-Nucleus NMR: 31 P and 19 F
Chem 636, Fall 2008 HW #9 Due at the beginning of lab, the week of Oct 28 (cgf: updated 12 July 2010) X-ucleus MR: 31 P and 19 F Many nuclei in MR can be detected in a manner similar to 13 C. 31 P and
More informationChapter 13: Nuclear Magnetic Resonance (NMR) Spectroscopy direct observation of the H s and C s of a molecules
hapter 13: Nuclear Magnetic Resonance (NMR) Spectroscopy direct observation of the s and s of a molecules Nuclei are positively charged and spin on an axis; they create a tiny magnetic field + + Not all
More informationTo Do s. Read Chapter 3. Complete the end-of-chapter problems, 3-1, 3-3, 3-4, 3-6 and 3-7. Answer Keys are available in CHB204H
Read Chapter 3. To Do s Complete the end-of-chapter problems, 3-1, 3-3, 3-4, 3-6 and 3-7 Answer Keys are available in CB204 NMR Chemical Shifts Further Discussion A set of spectral data is reported when
More informationNuclear Magnetic Resonance Parameters
Nuclear Magnetic Resonance Parameters P. K. Madhu Department of Chemical Sciences Tata Institute of Fundamental Research omi Bhabha Road Colaba Mumbai 400 005, India NMR: What are the Potentials? Understanding
More informationNuclear Magnetic Resonance Spectroscopy
Nuclear Magnetic Resonance Spectroscopy Features: Used to identify products of reactions Also gives information about chemical environment, connectivity and bonding of nuclei Requirements: Pure or mostly
More informationNMR Spectroscopy Laboratory Experiment Introduction. 2. Theory
1. Introduction 64-311 Laboratory Experiment 11 NMR Spectroscopy Nuclear Magnetic Resonance (NMR) spectroscopy is a powerful and theoretically complex analytical tool. This experiment will introduce to
More informationThree-Dimensional Triple-Resonance NMR of 13C / 15N-Enriched Proteins Using Constant-Time Evolution
JOURNAL OF MAGNETIC RESONANCE 94,209-2 13 ( 199 1) Three-Dimensional Triple-Resonance NMR of 13C / 15N-Enriched Proteins Using Constant-Time Evolution ROBERTPOWERS, ANGELA M. GRONENBORN,G.MARIUSCLORE,ANDADBAX
More informationNMR-spectroscopy of proteins in solution. Peter Schmieder
NMR-spectroscopy of proteins in solution Basic aspects of NMR-Spektroskopie Basic aspects of NMR-spectroscopy 3/84 Prerequisite for NMR-spectroscopy is a nuclear spin that can be thought of as a mixture
More informationBiophysical Chemistry: NMR Spectroscopy
Spin Dynamics & Vrije Universiteit Brussel 25th November 2011 Outline 1 Pulse/Fourier Transform NMR Thermal Equilibrium Effect of RF Pulses The Fourier Transform 2 Symmetric Exchange Between Two Sites
More informationNMR Spectroscopy of Polymers
UNESCO/IUPAC Course 2005/2006 Jiri Brus NMR Spectroscopy of Polymers Brus J 1. part At the very beginning the phenomenon of nuclear spin resonance was studied predominantly by physicists and the application
More informationBiochemistry 530 NMR Theory and Practice
Biochemistry 530 NMR Theory and Practice Gabriele Varani Department of Biochemistry and Department of Chemistry University of Washington Lecturer: Gabriele Varani Biochemistry and Chemistry Room J479 and
More informationTo Do s. Answer Keys are available in CHB204H
To Do s Read Chapters 2, 3 & 4. Complete the end-of-chapter problems, 2-1, 2-2, 2-3 and 2-4 Complete the end-of-chapter problems, 3-1, 3-3, 3-4, 3-6 and 3-7 Complete the end-of-chapter problems, 4-1, 4-2,
More informationChapter 13 Structure t Determination: Nuclear Magnetic Resonance Spectroscopy
John E. McMurry www.cengage.com/chemistry/mcmurry Chapter 13 Structure t Determination: ti Nuclear Magnetic Resonance Spectroscopy Revisions by Dr. Daniel Holmes MSU Paul D. Adams University of Arkansas
More informationThe Basics of Magnetic Resonance Imaging
The Basics of Magnetic Resonance Imaging Nathalie JUST, PhD nathalie.just@epfl.ch CIBM-AIT, EPFL Course 2013-2014-Chemistry 1 Course 2013-2014-Chemistry 2 MRI: Many different contrasts Proton density T1
More informationSlow symmetric exchange
Slow symmetric exchange ϕ A k k B t A B There are three things you should notice compared with the Figure on the previous slide: 1) The lines are broader, 2) the intensities are reduced and 3) the peaks
More informationNMR-spectroscopy. I: basics. Peter Schmieder
NMR-spectroscopy I: basics Why spectroscopy? 2/102 Why spectroscopy It is well established that all biological relevant processes take place via interactions of molecules, either small ones (metall ions,
More informationPhysical Background Of Nuclear Magnetic Resonance Spectroscopy
Physical Background Of Nuclear Magnetic Resonance Spectroscopy Michael McClellan Spring 2009 Department of Physics and Physical Oceanography University of North Carolina Wilmington What is Spectroscopy?
More informationAn Introduction to NMR Spectroscopy. The types of information accessible via high resolution NMR include:
1 of 40 An Introduction to NMR Spectroscopy 1 NMR 13C NMR The types of information accessible via high resolution NMR include: 1. Functional group analysis (chemical shifts) 2. Bonding connectivity and
More informationChemistry 416 Spectroscopy Fall Semester 1997 Dr. Rainer Glaser
Chemistry 416 Spectroscopy Fall Semester 199 Dr. Rainer Glaser First 1-Hour Examination NMR Spectroscopy Monday, October 6, 199, :40-9:0 Name: Answer Key Question 1 (Spectra) 20 Question 2 (Equivalence)
More informationTo Do s. Answer Keys are available in CHB204H
To Do s Read Chapters 2, 3 & 4. Complete the end-of-chapter problems, 2-1, 2-2, 2-3 and 2-4 Complete the end-of-chapter problems, 3-1, 3-3, 3-4, 3-6 and 3-7 Complete the end-of-chapter problems, 4-1, 4-2,
More informationStructure Determination: Nuclear Magnetic Resonance Spectroscopy
Structure Determination: Nuclear Magnetic Resonance Spectroscopy Why This Chapter? NMR is the most valuable spectroscopic technique used for structure determination More advanced NMR techniques are used
More information1H 1D-NOE Difference Spectra and Spin-Saturation Transfer Experiments on the GN500
UGN526 VVM-21JUN88CD VVM-31OCT91UD 1H 1D-NOE Difference Spectra and Spin-Saturation Transfer Experiments on the GN500 Double-resonance experiments are techniques which use a second irradiating field (B
More informationNuclear magnetic resonance spectroscopy II. 13 C NMR. Reading: Pavia Chapter , 6.7, 6.11, 6.13
Nuclear magnetic resonance spectroscopy II. 13 NMR Reading: Pavia hapter 6.1-6.5, 6.7, 6.11, 6.13 1. General - more/better/additional structural information for larger compounds -problems: a) isotopes
More informationTopics. The History of Spin. Spin. The concept of spin Precession of magnetic spin Relaxation
Topics Bioengineering 280A Principles of Biomedical Imaging Fall Quarter 2008 MRI Lecture 1 The concept of spin Precession of magnetic spin Relaation Spin The History of Spin Intrinsic angular momentum
More informationUNESCO - EOLSS SAMPLE CHAPTER
NMR SPECTROSCOPY Juan Carlos Paniagua and Miquel Pons University of Barcelona, Spain Keywords: chemical shift, correlation spectroscopy, diffusion coefficient, Fourier transform spectroscopy, imaging,
More informationBMB/Bi/Ch 173 Winter 2018
BMB/Bi/Ch 173 Winter 2018 Homework Set 8.1 (100 Points) Assigned 2-27-18, due 3-6-18 by 10:30 a.m. TA: Rachael Kuintzle. Office hours: SFL 220, Friday 3/2 4:00-5:00pm and SFL 229, Monday 3/5 4:00-5:30pm.
More informationIntroduction to Biomedical Imaging
Alejandro Frangi, PhD Computational Imaging Lab Department of Information & Communication Technology Pompeu Fabra University www.cilab.upf.edu MRI advantages Superior soft-tissue contrast Depends on among
More informationBASIC NMR HANDBOOK Written by M. A. Eastman Copyright 1997, 2001, 2013, 2015, 2018
BASIC NMR HANDBOOK Written by M. A. Eastman Copyright 1997, 2001, 2013, 2015, 2018 Basic NMR Handbook Table of Contents: Preface ii viii PART 1 Chapter 1: Introduction to NMR 1 Why Study NMR? 1 The Magnetic
More informationBiochemistry 530 NMR Theory and Practice
Biochemistry 530 NMR Theory and Practice Gabriele Varani Department of Biochemistry and Department of Chemistry University of Washington 1D spectra contain structural information.. but is hard to extract:
More informationNuclear Magnetic Resonance Imaging
Nuclear Magnetic Resonance Imaging Simon Lacoste-Julien Electromagnetic Theory Project 198-562B Department of Physics McGill University April 21 2003 Abstract This paper gives an elementary introduction
More informationLecture 02 Nuclear Magnetic Resonance Spectroscopy Principle and Application in Structure Elucidation
Application of Spectroscopic Methods in Molecular Structure Determination Prof. S. Sankararaman Department of Chemistry Indian Institution of Technology Madras Lecture 02 Nuclear Magnetic Resonance Spectroscopy
More informationMidterm Exam: CHEM/BCMB 8190 (148 points) Friday, 3 March, 2017
Midterm Exam: CHEM/BCMB 8190 (148 points) Friday, 3 March, 2017 INSTRUCTIONS: You will have 50 minute to work on this exam. You can use any notes or books that you bring with you to assist you in answering
More information10.3 NMR Fundamentals
10.3 NMR Fundamentals nuclear spin calculations and examples NMR properties of selected nuclei the nuclear magnetic moment and precession around a magnetic field the spin quantum number and the NMR transition
More informationSpectral Broadening Mechanisms. Broadening mechanisms. Lineshape functions. Spectral lifetime broadening
Spectral Broadening echanisms Lorentzian broadening (Homogeneous) Gaussian broadening (Inhomogeneous, Inertial) Doppler broadening (special case for gas phase) The Fourier Transform NC State University
More informationScott A. Smith and Nagarajan Murali 1
Journal of Magnetic Resonance 136, 27 36 (1999) Article ID jmre.1998.1582, available online at http://www.idealibrary.com on Relaxation Effects in a System of a Spin-1/2 Nucleus Coupled to a Quadrupolar
More information