Chem Portal
Phone Book
Careers
Contact
Search
Home
Research
Graduate Studies
Undergraduate Studies
News and Events
People
Alumni
Support Chemistry
Visuals for "Introduction to NMR": Undergraduate Lecture
These visuals are made from the original lecture transparencies
Nuclear Magnetic Resonance: Spin, Field, Precession
Classical vs Quantum
NMR Active Nuclei
Cycloheptanone
13
C Spectrum at 50 MHz
Origin of the Chemical Shift
Cartoon Diagram of an NMR Spectrometer
Pulsed Fourier Transform: the Piano Experiment
Tuning of Bells
The Free Induction Decay (FID)
Simple 1D Acquisition: Relax, Pulse, FID
Signal Averaging: Four Transients
NMR Hardware: Simple Block Diagram of an NMR Spectrometer
Chemical Shift: A Result of the Local Magnetic Environment
Chart of
1
H and
13
C Chemical Shifts for Organic Functional Groups
The J Coupling Interaction
Physical Basis of Spin-Spin Coupling
Multiple Splitting: Triplet and Quartet
Complex Splitting (Spin-1/2 Nuclei): dt and ddd
NOE: A Through-Space Interaction
Solvents for
1
H NMR
Equivalence in NMR
Integration: Peak Areas
1
H NMR Example: 4-isopropylacetophenone
13
C NMR Example: 4-isopropylacetophenone
Fluxional Molecules: The NMR Time Scale
Analytical Services Group
Electron Paramagnetic Resonance Spectroscopy (EPR)
Electron Spectroscopy and Surface Analysis (LESSA)
W.M. KECK Imaging Center (KECK)
Clean Room
Mass Spectrometry (MS)
Nuclear Magnetic Resonance Spectroscopy (NMR)
Instrumentation
Instructional Manuals
NMR Courses
NMR Training
Photoelectron Spectroscopy (PES)
Proteomics
X-ray Diffraction (XDF)
Design Group
Chemical Synthesis (CSF)
Computing and Graphics (CGF)
Glass Shop
Instrumentation and Electronics (ChIEF)
Machine Shop
NMR Training Lecture Transparencies:
Please select the Article you would like to view from the drop down list:
Wednesday, June 2, 2004
The Rules
Sample Preparation
Sample Depth
The Deuterium Lock Channel
Lock Circuit Feedback Loop
Lock Display
Diagram of Z Shims and B
o
Inhomogeneity
Interaction of Z1 and Z2 Shims
Bad Z2 Shim: Sucrose
1
H Spectrum
Receiving the FID: Block Diagram
FID: CHCl
3
/CH
2
Cl2, 0 to 2 9 seconds
FID: CHCl
3
/CH
2
Cl2, 0 to 0 425 seconds
FID: CHCl
3
/CH
2
Cl2, 0 to 36 ms
Digitization of the FID
Limits of Digitization: the Nyquist Theorem
Quadrature Detection: Cartoon Model
Digitized FID Data (DW = 80 microseconds)
FID: CHCl
3
/CH
2
Cl
2
, 0 to 36 ms, Analyzed
Spectrum: CHCl
3
/CH
2
Cl
2
, with MHz, Hz and ppm Scales
Folding or Aliasing
Acquisition Parameters: Relationship of SW, AT and NP
Sum to Memory
Receiver Gain Optimization
***********************************************************************************************************
Thursday, June 3, 2004
Window (Multiplier) Functions
Raw FID Data and Exponential Multiplier Function
FID Data Before and After Exponential Multiplication
Spectrum With and Without Exponential Multiplication
FID: CHCl
3
/CH
2
Cl
2
, 0 to 2.9 seconds, after Exponential Multiplication
Spectrum: CHCl
3
/CH
2
Cl
2
with LB = 0.2 Hz vs 2.0 Hz
Phase: Dispersive and Absorptive Peak Shapes
Phase Correction: Linear Combination of Real and Imaginary Spectra
Phase Correction with a Hypothetical Spectrum: Zero and First Order Terms
Phase Twist and How to Avoid It
***********************************************************************************************************
Monday, June 16, 2008
Room 122 Old Chemistry: Layout of NMR and Computers
Cockpit of the Unity-300
Interface between Sun and Varian
VNMR Screen Layout
Parameter and Peak List from VNMR
The Spectral Window
VNMR Parameters
VNMR Commands
UNIX Operating System
Variable Temperature Unit
1D
1
H Spectrum of Cholesterol
Pulse Width = Duration in microseconds
Arrayed Experiments
Calibration of 90
o
13
C Pulse
Physical Basis of Spin-Spin Coupling
13
C Satellites of CHCl
3
13
C spectrum of phenetole, dm=yyn
13
C spectrum of sucrose, coupled and decoupled
Coupling and decoupling: theory
Varian hardware setup for decoupling
Varian "status" parameter
13
C spectrum of phenetole, dm=nny
13
C spectrum of phenetole, dm=yyy
13
C decoupling modes: summary
The Next Step: DEPT
***********************************************************************************************************
Tuesday, June 17, 2008
The Next Step: DEPT
DEPT
LGJC4:
13
C, DEPT-90 and DEPT-135 Stacked Plot
Cholesterol pure subspectra: CH, CH
2
and CH
3
vs
Sensitivity comparison: APT and
13
C vs DEPT
NOE difference: pulse sequence diagram
Hardware Setup for NOE Difference and Homo. Decoupling
Interleaved acquisition: array of dof values
Steady-state NOE: heat transfer analogy
NOE difference: Sucrose H-g1
NOE difference: Sucrose H-f1
NOE difference: Cholesterol H4ab
***********************************************************************************************************
Thursday, June 26, 2008
The High-Field Advantage
1
H Spectrum of Menthol at 200, 250, 300, 500 and 600 MHz (Hz Scale)
1
H Spectrum of Menthol at 200, 250, 300, 500 and 600 MHz (ppm Scale)
Evolution of Bruker NMR Spectrometers
New Capabilities of the DRX-500 Console
Digital Filters: Frequency Response Compared to Analog Filters
Oversampling and Digital Filtering: Receiver Block Diagram
Photo of Bruker Avance DRX-500 Console and Computer
Photo of Bruker Avance DRX-500 Console and Magnet
What We Keep and What We Replace in Console Upgrade
Photo of DRX-500 Console with Doors Open
Diagram of DRX-500 Console with Doors Open
Block Diagram of 3-Channel DRX Spectrometer
Photo of Computer
Diagram of BSMS Keyboard
Photo of BSMS Keyboard
Diagram of Preamplifier Stack
Photo of Base of Magnet
Close-Up Photo of Dual Probe
Close-Up Photo of Dual Probe, Side View
Close-Up Photo of Nalorac Probe
Close-Up Photo of Nalorac Probe, Side View
Tuning the Probe
Photo of Monitor Showing Wobb Display
What is the "excitation profile" of a pulse?
Gaussian pulse as a laminar pulse
Selective Gaussian Pulse on Sucrose at Different Frequencies
Pulsed field gradients - profile of NMR tube
Gradient pulse leads to twisted coherence
Untwisting the coherence
Lock Signal in Gradient Experiments
XWinNMR Software
UNIX Operating System: Bruker Data Structure
***********************************************************************************************************
Tuesday, July 8, 2008
Advanced 1D Experiments
NOE difference: pulse sequence diagram
Steady-state NOE: heat transfer analogy
NOE difference: Cholesterol H4ab
Transient NOE: Heat flow analogy
Transient NOE: z-magnetization vs time
What is the "excitation profile" of a pulse?
Selective Gaussian pulse on Sucrose at Different Frequencies
Pulsed field gradients - on vs off
Gradient pulse leads to twisted coherence
Gradient Echo
Untwisting the coherence
Effect of 180
o
pulse on twisted coherence
Gradient-enhanced spin-echo
Gradient-enhanced spin-echo: Selected Magnetization
Gradient-enhanced spin-echo: Other (non-selected) Magnetization
Selective 1D Transient NOE: A J Shaka
500 MHz
1
H spectrum of cholesterol: H4eq and H4ax signals
Selective 1D NOE: results for H4eq (top) and H4ax (bottom)
Transient NOE buildup curves for Sucrose H-f1 to H-g1 and H-f3
TOCSY 2D vs TOCSY 1D: pulse sequences
TOCSY: spin systems and downfield "handles"
TOCSY: how far can you go?
Selective 1D TOCSY: pulse sequence using PFGSE
Results: selecting sucrose H-g1
Results: selecting cholesterol H3 (top) and H6 (bottom)
General Setup Procedure for DRX-500
***********************************************************************************************************
Tuesday, July 15, 2008
2-D Spectrum: a matrix of data values
Display of 2D Data
Transfer of Magnetization: Mixing
General Pulse Sequence for 2D Experiments
Diagram of evolution during t
1
and t
2
periods: nth t
1
value
Diagram of evolution during t
1
and t
2
periods: (n+1)th t
1
value
Diagram of evolution during t
1
and t
2
periods: (n+2)th t
1
value
Diagram of evolution during t
1
period
The t
1
FID
2D Data Matrix: after F
2
Fourier transform
2D Spectrum: after F
1
Fourier transform
Summary of 2D NMR Experiments
2D Connections (Shift Correlation)
HETCOR (Heteronuclear Correlation)
2-D HETCOR: diagram for transfer of magnetization
HETCOR spectrum of sucrose
Comparison of HMQC and HETCOR
HMQC / HSQC: overview
HMQC/HSQC vs. HMBC
Cartoon of 2D spectrum without
13
C decoupling
HMQC Spectrum of 3-Heptanone without
13
C Decoupling
HMQC spectrum of sucrose in D
2
O : no
13
C decoupling
HMQC spectrum of sucrose in D
2
O : no
13
C decoupling, with
1
J
CH
values
HMQC of sucrose: non-anomeric CH region
HMQC of cholesterol without
13
C decoupling: methyl region
HSQC pulse sequence (simplified)
Gradient-Enhanced HSQC: 3 gradient pulses
Gradient-Enhanced HSQC: 2 gradient pulses
Edited Decoupled HSQC
13
C-decoupled HSQC of sucrose in D
2
O (500 MHz, gradients)
Decoupled Edited HSQC of Testosterone Metabolite "product 2"
HSQC of Testosterone Metabolite "product 2": upfield region
HSQC of Testosterone Metabolite "product 2": upfield region with assignments
HSQC of Testosterone Metabolite "product 2": upfield region with stereospecific assignments
***********************************************************************************************************
Wednesday, July 16, 2008
Gradient pulse leads to twisted coherence
Gradient-Enhanced HSQC: 3 gradient pulses
General Setup Procedure for DRX-500
The 2D Spectral Window: Bruker Parameters
2D NMR Parameters: Bruker
Window Functions for 2D NMR: Bruker Parameters
Menu Display after eda Command (Page 1)
Menu Display after eda Command (Page 2)
Menu Display after edp Command
Interactive 2D Phase Correction
Cholesterol
1
H and
13
C Spectra Arranged on x and y Axes
Cholesterol
1
H and
13
C Spectra with Two HSQC Crosspeaks
Expansion of Downfield Region: Cholesterol HSQC with 1D Spectra
Cholesterol HSQC Spectrum with
1
H and
13
C Spectra
Cholesterol HSQC Spectrum
Expansion of Upfield Region: Cholesterol HSQC with 1D Spectra
Edited
13
C-Decoupled HSQC of Cholesterol
F
2
slices at carbons j, q and s of Cholesterol HSQC
HSQC / HMQC and HMBC
One-bond vs 2-3 bond correlations
13
C-decoupled HSQC of sucrose in D
2
O (500 MHz, gradients)
HMBC of sucrose in D
2
O
HMBC of sucrose in D
2
O, with overlay of HSQC spectrum
HMBC of sucrose in D
2
O, with diagram of 2 and 3 bond correlations
HMBC of sucrose in D
2
O: upfield region
HSQC Spectrum of Product 2: Expanded Region
1D
1
H Spectrum of Product 2: Two expansions (overlay)
HMBC Spectrum of Product 2: Expanded Region (overlay)
Conformational Effects in HMBC
COSY and DQF-COSY
Homonuclear Shift Correlation: COSY
3-heptanone in CDCl
3
: DQF-COSY Spectrum 600 MHz
3-heptanone: DQF-COSY with H1-H2 Spin System
3-heptanone: DQF-COSY with H4-H5-H6-H7 Spin System
3-heptanone: DQF-COSY with Assignments and Correlation Diagram
3-heptanone: DQF-COSY showing artifacts
DQF-COSY Spectrum of Sucrose (Full Matrix)
300 MHz COSY Spectrum of Sucrose: Full Spectrum
DQF-COSY Spectrum of Sucrose: H(g1) - H(g2) Crosspeak Fine Structure
300 MHz COSY Spectrum of Sucrose: Upfield Region
600 MHz COSY Spectrum of Sucrose: Upfield Region
Double-Quantum Filtered COSY
Coherence pathway selection using gradients
TOCSY overview
3-heptanone in CDCl
3
: Simulated TOCSY Spectrum
3-heptanone in CDCl
3
: TOCSY Spectrum 72 ms mixing 600 MHz
3-heptanone in CDCl
3
: Overlay for TOCSY Spectrum
TOCSY of Heregulin-alpha
NOESY overview
Gradient-Enhanced NOESY
Measurement of crosspeak volumes (sucrose NOESY)
NOESY Spectrum of Unknown F
NOESY Correlations for Unknown F,
13
C Spectrum of Unknown F
Maximum Theoretical Overhauser Effect
The Spin-Lock
ROESY Pulse Sequence Diagram
ROESY of Pristimerin Oxidation Product, olefinic to upfield
ROESY of Pristimerin Oxidation Product, olefinic to upfield, with Structure Diagram
Pristimerin Oxidation Product Structure with Distances and
1
H Spectrum
***********************************************************************************************************