Name: nmr peak shape and magnetic field shimming
Uploaded: 2024-04-04T10:51:41.000Z
Duration: 1 min 14 s
Channel: JoVE

NMR 스펙트럼의 로렌츠 피크는 위치, 진폭 및 최대 절반에서의 전체 너비로 정의됩니다.
완벽하게 균질한 필드에서 적절하게 준비된 샘플의 피크 너비는 스핀-스핀 이완 시간에만 의해 제어됩니다.
그러나, 적용된 자기장 B0는 샘플과 프로브의 존재에 의해 불균일하게 됩니다. 그 결과 외부 측대역과 낮은 분해능으로 피크가 넓어집니다.
자기장의 불균일성은 시밍(shimming)이라는 과정에 의해 수정됩니다.
shimming 동안 전류는 프로브를 둘러싼 심 코일 세트를 통해 통과하여 샘플 근처에서 B0를 강화하거나 반대하는 작은 자기장을 생성합니다.
이러한 심 코일 자기장은 샘플 전체에서 가장 균일한 자기장을 얻기 위해 조작됩니다.
최적화된 펄스 시퀀스 파라미터 및 적절한 시료 준비와 함께 시밍은 우수한 피크 모양, 높은 신호 대 잡음비 및 최대 분해능을 보장합니다.

nmr 분광계: 분해능 및 오류 수정

NMR Spectrometers: Resolution and Error Correction

샘플의 자기 핵이 공명을 이루고 이완을 겪을 때 NMR에서 감지된 신호는 대략 지수적 자유 유도 붕괴입니다. 지수 감쇠의 푸리에 변환은 주파수 영역에서 로렌츠 피크를 생성합니다. NMR 스펙트럼의 로렌츠 피크는 진폭, 최대 반치에서의 전체 폭, 위치에 의해 정의됩니다. 여기서 피크 폭은 스핀-스핀 완화 시간에만 영향을 받습니다. 그러나 실제 실험에서는 적용된 자기장이 샘플과 프로브의 존재로 인해 불균일하게 렌더링되어 외부 측파대와 열악한 분해능으로 피크가 넓어집니다.

이러한 불균일성은 시밍이라는 프로세스를 통해 스펙트럼이 기록되기 전에 수정됩니다. 심 코일 세트는 프로브를 둘러싸고 통과하는 전류에 따라 작은 자기장을 생성합니다. 이러한 필드는 샘플 근처에서 B0를 강화하거나 반대할 수 있습니다. 시밍에는 샘플 전체에서 가장 균일한 자기장을 얻기 위해 코일장을 조작하여 불균일성을 수정하는 작업이 포함됩니다. 시밍, 최적화된 펄스 시퀀스 매개변수 및 적절한 샘플 준비를 통해 우수한 피크 모양, 낮은 신호 대 잡음비 및 최대 분해능이 보장됩니다.

NMR 분광계: 분해능 및 오류 수정

샘플의 자기 핵이 공명을 달성하고 이완을 겪을 때 NMR에서 감지된 신호는 대략 기하급수적인 자유 유도입니다.

nmr-spectrometers-resolution-and-error-correction

Education

교육

JoVE Core

Analytical Chemistry

분석 화학

Unit 1

제1단원

Principles of Nuclear Magnetic Resonance

핵자기공명 원리

KEY TERMS AND CONCEPTS

주요 용어 및 개념

nmr peak shape and magnetic field shimming

NMR peak shape depends on the signal created after magnetic nuclei resonate and relax. The detected free induction decay is approximately exponential. When that decay is Fourier transformed, it becomes a Lorentzian peak in the frequency domain.

A Lorentzian peak in an NMR spectrum is described by its amplitude, full width at half maximum, and position. Its width is governed by the spin-spin relaxation time alone. In real experiments, the sample and probe can make the magnetic field inhomogeneous. This can broaden peaks, add side-bands, and reduce resolution.

These field problems are corrected before spectra are recorded by shimming. Shim coils surround the probe and produce small magnetic fields based on the current applied to them. Their fields can either enhance or oppose B0 near the sample. By adjusting the coil fields, shimming makes the magnetic field more uniform across the sample.

Good shimming works best with optimized pulse sequence parameters and proper sample preparation. Together, these steps help produce good peak shape, low signal-to-noise ratio, and maximum resolution in NMR spectra.

NMR Peak Shape and Magnetic Field Shimming

nmr-peak-shape-and-magnetic-field-shimming

nuclear magnetic resonance (nmr): overview

NMR Spectra and MRI Imaging

Nuclear magnetic resonance, or NMR, is a phenomenon that certain nuclei can show when they absorb radio frequency energy under the right conditions. Scientists use it in molecular spectroscopy and in medical imaging. In both cases, the sample or the person being studied is placed in a magnetic field and exposed to radio frequency energy. In NMR spectroscopy, the result is a spectrum. This spectrum plots the absorption frequencies of the sample against peak intensity. The pattern gives detailed...

atomic nuclei: nuclear spin

Nuclear Spin and NMR-Active Nuclei

Atomic nuclei have nuclear spin, which comes from the spins of their protons and neutrons. These particle spins are intrinsic angular momentum, and each electron, proton, and neutron has a spin value of 1/2. In nuclei, proton spins pair with other protons, and neutron spins pair with other neutrons. They do not pair with each other, so the final nuclear spin depends on which nucleons are left unpaired. Even numbers of protons do not add to the nuclear spin, and even numbers of neutrons do not...

atomic nuclei: nuclear magnetic moment

Nuclear Spin States and Magnetic Alignment

Atomic nuclei can act like tiny magnets when they have a nonzero spin. Because they are positively charged and rotating, they generate a magnetic field and a magnetic moment. In the absence of an external magnetic field, this magnetic moment points in random directions. When an external magnetic field, B0, is applied, the nuclear magnetic moments can line up with the field or against it. These two directions create 2I + 1 orientations. A hydrogen nucleus is a proton, and it has spin 1/2, so it...

atomic nuclei: nuclear spin state overview

atomic-nuclei-nuclear-spin-state-overview

Zeeman Splitting in Nuclear Spin States

NMR-active nuclei have spin states that describe the orientation of their nuclear magnetic moments. Without a magnetic field, these moments point in random directions, and the spin states are degenerate, meaning they have the same energy. When an external magnetic field is applied, the nucleus can only take on 2I + 1 orientations, where I is the nuclear spin. A proton with spin 1/2 has two possible orientations. A quadrupolar nucleus with spin 1 has three possible orientations. The...

atomic nuclei: nuclear spin state population distribution

atomic-nuclei-nuclear-spin-state-population-distribution

Nuclear Spin Populations and NMR Signal

Nuclear spin populations help explain why NMR signals appear. In a magnetic field, nuclei can occupy a lower energy spin-up state or a higher energy spin-down state. Near absolute zero, most nuclei stay in the lower energy state. As temperature rises, thermal collisions spread the spins more evenly between the two states. The balance between the spin −1/2 and spin +1/2 populations is described by the Boltzmann distribution equation. In this equation, ΔE is the energy difference, k is the...

atomic nuclei: larmor precession frequency

atomic-nuclei-larmor-precession-frequency

Magnetic Field and Nuclear Precession

Magnetic field strength controls nuclear precession in NMR. A spinning nucleus has a magnetic moment, and that moment turns around an external magnetic field directed along the z-axis. This motion is called Larmor precession, and its angular frequency is the Larmor frequency. The Larmor frequency is directly proportional to the applied magnetic field, B0. The proportionality constant is the gyromagnetic ratio, gamma. This value is fixed for each nucleus because every nucleus has its own ratio...

atomic nuclei: magnetic resonance

Nuclear Spins and Resonance in a Magnetic Field

Nuclear spins can line up in a magnetic field and create nuclear magnetic resonance. In the lower energy state, slightly more spins are aligned than in the higher energy state. That small difference gives the nuclei a net magnetization along the z axis.

atomic nuclei: nuclear relaxation processes

atomic-nuclei-nuclear-relaxation-processes

Nuclear Spin Alignment and Relaxation

Nuclear spin alignment and relaxation describe how nuclear spins respond to a magnetic field and then return to equilibrium. Without an external magnetic field, nuclear spin states are degenerate, meaning they have the same energy, and the spins are randomly oriented. When a magnetic field is applied, the spins begin to precess, or wobble, and orient themselves either along the field in a lower energy state or against it in a higher energy state. At equilibrium, a slight excess of spins...

atomic nuclei: types of nuclear relaxation

atomic-nuclei-types-of-nuclear-relaxation

NMR Relaxation Paths in Atomic Nuclei

Nuclear relaxation in atomic nuclei helps restore the balance between energy levels in NMR systems. It occurs through two main paths: spin-lattice relaxation and spin-spin relaxation. Both are first-order exponential decay processes. Spin-lattice relaxation is also called longitudinal relaxation. In this process, excited spins give energy to the surrounding lattice as they move back to the lower energy level. Magnetic dipolar interactions are an important part of this mechanism. A common...

nmr spectrometers: overview

How NMR Spectrometers Record Signals

NMR spectrometers record signals from samples that contain NMR-active nuclei. The system uses a strong magnet, a radiofrequency transmitter, and a detector connected to a computer console. These parts work together to measure and display the spectrum of the sample. Early NMR instruments were continuous-wave spectrometers. In a frequency-sweep method, the magnetic field stays fixed while the rf signal is swept. In a field-sweep method, the radiofrequency signal stays fixed while the magnetic...

nmr spectrometers: radiofrequency pulses and pulse sequences

nmr-spectrometers-radiofrequency-pulses-and-pulse-sequences

NMR Pulse Angles and Signal Collection

NMR pulse angles and signal collection explain how radiofrequency energy starts a measurement. A pulse is a short burst of radio waves spread across a range of frequencies. It excites the nuclei in the sample at the same time. When a radiofrequency pulse is applied along the x-axis, nuclei absorb energy that matches their Larmor frequencies and reach resonance. The net magnetization vector moves away from the z-axis and toward the transverse plane. This rotation angle is called the flip angle.

nmr spectrometers: resolution and error correction

NMR peak shape depends on the signal created after magnetic nuclei resonate and relax. The detected free induction decay is approximately exponential. When that decay is Fourier transformed, it becomes a Lorentzian peak in the frequency domain. A Lorentzian peak in an NMR spectrum is described by its amplitude, full width at half maximum, and position. Its width is governed by the spin-spin relaxation time alone. In real experiments, the sample and probe can make the magnetic field...

diamagnetic shielding of nuclei: local diamagnetic current

diamagnetic-shielding-of-nuclei-local-diamagnetic-current

How Electron Density Shields Nuclei in NMR

Electron density around a nucleus affects how strongly it is shielded in NMR spectroscopy. When an applied magnetic field acts on a molecule, the electrons begin to circulate. This creates a local diamagnetic current within the molecule. The circulating sigma-bonding electrons produce a local magnetic field, B local, that opposes the applied field, B0. The nucleus then feels an effective magnetic field, which is the difference between the applied field and the local field. This effect is...

key terms and concepts

Learn how NMR peak shape forms, why field inhomogeneity broadens signals, and how shimming improves resolution with better magnetic field uniformity.

NMR Peak Shape and Magnetic Field Shimming | JoVE K12

analytical chemistry

JoVE Core Analytical Chemistry simplifies complex chemical principles by breaking them down into clear, engaging animations, making topics from SI Units to NMR spectroscopy more accessible and straightforward. Additionally, the scientist-in-action videos highlight the application of these concepts in real-world research conducted in laboratories globally.

NMR Peak Shape and Magnetic Field Shimming

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