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2024 | Book

Optimising NMR Spectroscopy Through Method and Software Development

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About this book

This book provides a comprehensive overview of Nuclear Magnetic Resonance (NMR) theory, its applications, and advanced techniques to improve the quality and speed of NMR data acquisition. In this book, the author expands his outstanding Ph.D. thesis and provides a valuable resource for researchers, professionals, and students in the field of NMR spectroscopy.

The book covers quantum mechanics basics, and topics like density operators, pulse sequences, 1D pulse acquisition, INEPT (Insensitive nuclei enhancement by polarization transfer), product operators, and 2D NMR principles. It also explores innovative experiments like States HSQC (Heteronuclear Single Quantum Coherence) and echo-antiecho HSQC with gradients.

In the subsequent chapters, the author discusses Pure Shift NMR, including PSYCHE (Pure Shift Yielded by Chirp Excitation) and its optimizations, such as waveform parameterization and time-reversal methods. The 'Discrete PSYCHE' approach and Ultrafast PSYCHE-iDOSY (Diffusion-ordered spectroscopy) are also highlighted.

This book presents the POISE (Parameter Optimisation by Iterative Spectral Evaluation) software for real-time NMR experiment optimization, including pulse width calibration and Ernst angle optimization, and demonstrates applications across various NMR experiments.

Lastly, the book examines accelerated 2D NMR data collection and the NOAH (NMR by Ordered Acquisition using 1H detection) supersequences, emphasizing automated pulse program creation using GENESIS (GENEration of Supersequences In Silico). Covered NMR experiments include 13C sensitivity-enhanced HSQC, 15N HMQC (Heteronuclear Multiple Quantum Coherence), dual HSQC, HSQC-TOCSY (Total Correlation Spectroscopy), HMBC (Heteronuclear Multiple Bond Correlation), and ADEQUATE (Adequate Sensitivity Double-Quantum Spectroscopy).

Table of Contents

Frontmatter
Chapter 1. NMR Theory
Abstract
In the opening chapter of this thesis, I provide an overview of basic NMR theory, specifically, the dynamics of quantum systems containing one or more spin-\(\frac{1}{2}\) particles. Starting from the Schrödinger equation, I progressively develop the rotating frame and density operator formalisms used in the analysis and simulation of simple NMR experiments. The important product operator formalism, used throughout this thesis, is exemplified through a selection of 1D and 2D experiments. Since 2D experiments form a very large part of this thesis, I also discuss a number of general principles in 2D NMR.
Jonathan Yong
Chapter 2. Pure Shift NMR
Abstract
Pure shift NMR refers to the technique of acquiring broadband homodecoupled NMR spectra, where all multiplet structure is suppressed and each chemical environment gives rise to a singlet [1, 2]. Here, ‘broadband’ means that the couplings are removed from the entire spectrum, and ‘homodecoupled’ refers to the removal of homonuclear couplings: unlike heteronuclear couplings, these cannot be removed by applying RF pulses during the acquisition period, as that will destroy the desired signal itself.
Jonathan Yong
Chapter 3. POISE
Abstract
This chapter describes the development of a piece of software for on-the-fly optimisation of NMR experimental parameters, titled POISE (Parameter Optimisation by Iterative Spectral Evaluation). POISE is primarily written in Python 3 and includes an interface to Bruker’s TopSpin software, allowing optimisations to be started directly from the TopSpin command line. Through this optimisation process, NMR acquisition parameters can be adjusted for individual spectrometers and samples, ultimately leading to improved spectral quality.
Jonathan Yong
Chapter 4. NOAH
Abstract
This final chapter describes my work on NOAH (NMR by Ordered Acquisition using \({}^{1}\mathrm{{H}}\) detection) supersequences, pulse sequences which record multiple 2D datasets (‘modules’) in the time required for one. This is an attractive NMR technique for several reasons: the time savings are clearly a key factor, but the flexibility of being able to combine almost any set of modules also makes NOAH supersequences applicable to a variety of contexts.
Jonathan Yong
Backmatter
Metadata
Title
Optimising NMR Spectroscopy Through Method and Software Development
Author
Jonathan Yong
Copyright Year
2024
Electronic ISBN
978-3-031-46684-7
Print ISBN
978-3-031-46683-0
DOI
https://doi.org/10.1007/978-3-031-46684-7