Introduction to NMR - Undergraduate Lecture:

•    Nuclear Magnetic Resonance: Spin, Field, Precession
•    Classical vs Quantum
•    Cycloheptanone ¹³C 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 ¹H and ¹³C 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 ¹H NMR
•    Equivalence in NMR
•    Integration: Peak Areas
•    ¹H NMR Example: 4-isopropylacetophenone
•    ¹³C NMR Example: 4-isopropylacetophenone
•    Fluxional Molecules: The NMR Time Scale

Basic NMR Training Workshop Lecture I:

•    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 ¹H Spectrum
•    Receiving the FID: Block Diagram
•    FID: CHCl₃/CH₂Cl2, 0 to 2 9 seconds
•    FID: CHCl₃/CH₂Cl2, 0 to 0 425 seconds
•    FID: CHCl₃/CH₂Cl2, 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: CHCl₃/CH₂Cl₂, 0 to 36 ms, Analyzed
•    Spectrum: CHCl₃/CH₂Cl₂, with MHz, Hz and ppm Scales
•    Folding or Aliasing
•    Acquisition Parameters: Relationship of SW, AT and NP
•    Sum to Memory
•    Receiver Gain Optimization

Basic NMR Training Workshop Lecture II:

•    Window (Multiplier) Functions
•    Raw FID Data and Exponential Multiplier Function
•    FID Data Before and After Exponential Multiplication
•    Spectrum With and Without Exponential Multiplication
•    FID: CHCl₃/CH₂Cl2, 0 to 2 9 seconds
•    FID: CHCl₃/CH₂Cl₂, 0 to 2.9 seconds, after Exponential Multiplication
•    Spectrum: CHCl₃/CH₂Cl₂ 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

Varian Unity-300 Training Workshop Lecture I:

•    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 ¹H Spectrum of Cholesterol
•    Pulse Width = Duration in microseconds
•    Arrayed Experiments
•    Calibration of 90^{o 13}C Pulse
•    Physical Basis of Spin-Spin Coupling
•    ¹³C Satellites of CHCl₃
•    ¹³C spectrum of phenetole, dm=yyn
•    ¹³C spectrum of sucrose, coupled and decoupled
•    Coupling and decoupling: theory
•    Varian hardware setup for decoupling
•    Varian "status" parameter
•    The heteronuclear NOE
•    ¹³C spectrum of phenetole, dm=yyy
•    ¹³C spectrum of phenetole, dm=nny
•    ¹³C decoupling modes: summary
•    The Next Step: DEPT

Varian Unity-300 Training Workshop Lecture II:

•    The Next Step: DEPT
•    DEPT
•    LGJC4: ¹³C, DEPT-90 and DEPT-135 Stacked Plot
•    Cholesterol pure subspectra: CH, CH₂ and CH₃ vs
•    Sensitivity comparison: APT and ¹³C vs DEPT
•    Sensitivity comparison: APT and ¹³C vs DEPT, Expanded
•    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

Bruker DRX-500 Training Workshop Lecture I:

•    The High-Field Advantage
•    ¹H Spectrum of Menthol at 200, 250, 300, 500 and 600 MHz (Hz Scale)
•    ¹H 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

Bruker DRX-500 Training Workshop Lecture II:

•    Advanced 1D Experiments
•    NOE difference: pulse sequence diagram
•    Steady-state NOE: heat transfer analogy
•    NOE difference: Sucrose H-g1
•    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 ¹H 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

Bruker DRX-500 Training Workshop Lecture III:

•    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 t₁ and t₂ periods: nth t₁ value
•    Diagram of evolution during t₁ and t₂ periods: (n+1)th t₁ value
•    Diagram of evolution during t₁ and t₂ periods: (n+2)th t₁ value
•    Diagram of evolution during t₁ period
•    The t₁ FID
•    2D Data Matrix: after F₂ Fourier transform
•    2D Spectrum: after F₁ 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 ¹³C decoupling
•    HMQC Spectrum of 3-Heptanone without ¹³C Decoupling
•    HMQC spectrum of sucrose in D₂O : no ¹³C decoupling
•    HMQC spectrum of sucrose in D₂O : no ¹³C decoupling, with ¹J_CH values
•    HMQC of sucrose: non-anomeric CH region
•    HMQC of cholesterol without ¹³C decoupling: methyl region
•    HSQC pulse sequence (simplified)
•    Gradient-Enhanced HSQC: 3 gradient pulses
•    Gradient-Enhanced HSQC: 2 gradient pulses
•    Edited Decoupled HSQC
•    ¹³C-decoupled HSQC of sucrose in D₂O (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

Bruker DRX-500 Training Workshop Lecture IV:

•    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 ¹H and ¹³C Spectra Arranged on x and y Axes
•    Cholesterol ¹H and ¹³C Spectra with Two HSQC Crosspeaks
•    Expansion of Downfield Region: Cholesterol HSQC with 1D Spectra
•    Cholesterol HSQC Spectrum with ¹H and ¹³C Spectra
•    Cholesterol HSQC Spectrum
•    Expansion of Upfield Region: Cholesterol HSQC with 1D Spectra
•    Edited ¹³C-Decoupled HSQC of Cholesterol
•    F₂ slices at carbons j, q and s of Cholesterol HSQC
•    HSQC / HMQC and HMBC
•    One-bond vs 2-3 bond correlations
•    ¹³C-decoupled HSQC of sucrose in D₂O (500 MHz, gradients)
•    HMBC of sucrose in D₂O
•    HMBC of sucrose in D₂O, with overlay of HSQC spectrum
•    HMBC of sucrose in D₂O, with diagram of 2 and 3 bond correlations
•    HMBC of sucrose in D₂O: upfield region
•    HSQC Spectrum of Product 2: Expanded Region
•    1D ¹H 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 CDCl₃: 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 CDCl₃: Simulated TOCSY Spectrum
•    3-heptanone in CDCl₃: TOCSY Spectrum 72 ms mixing 600 MHz
•    3-heptanone in CDCl₃: 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, ¹³C 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 ¹H Spectrum

Chem 528 Lecture: NMR as an Analytical Tool

•    NMR vs. Mass Spectrometry
•    Photo of Fuel Additive Bottle (1)
•    Photo of Fuel Additive Bottle (2)
•    Components of Fuel Additive Determined by NMR and MS
•    ¹³C Assignments of Fuel Additive Mixture
•    ¹H Assignments of Fuel Additive Mixture
•    ¹³C Spectrum of Fuel Additive Mixture: CO region
•    ¹³C Spectrum of Fuel Additive Mixture: upfield region
•    2D HSQC Spectrum of Fuel Additive Mixture
•    2D HMBC Spectrum of Fuel Additive Mixture