Name: how nmr spectrometers record signals
Uploaded: 2024-04-04T10:51:41.000Z
Duration: 1 min 20 s
Channel: JoVE

NMR分光計は、強力な磁石、高周波またはRF送信機、およびコンピューターコンソールに取り付けられた検出器で構成されています。
連続波分光計と呼ばれる第1世代のNMR機器は、周波数スイープ法またはフィールドスイープ法を使用してスペクトルを記録します。
共振周波数は、前者では磁場強度を固定し、rf信号を変化させることによって決定されますが、後者では磁場強度が掃引されます。
最新のパルスフーリエ変換NMRまたはFT-NMR装置では、磁場は一定に保たれ、サンプルには一連の短い高出力RFパルスが照射されます。
パルスは大きな周波数拡散を持ち、さまざまな共鳴周波数でNMR活性核を同時に励起することができます。
パルス間の間隔または遅延により、原子核は弛緩して元の状態に戻り、自由誘導崩壊またはFID信号の形でrfエネルギーを放出します。
検出器によって記録されたFID信号は、フーリエ変換によって周波数対振幅信号、つまりNMRスペクトルに変換されます。

nmr 分光計: 概要

NMR Spectrometers: Overview

NMR 分光計は、強力な磁石、高周波送信機、および NMR 活性核を含むサンプルのスペクトルを記録するためにコンピューター コンソールに取り付けられた検出器で構成されています。連続波分光計と呼ばれる第一世代の NMR 装置では、原子核の共鳴周波数は周波数掃引法または磁場掃引法によって決定されます。前者では磁場強度が固定され、RF（無線周波数）信号が掃引されます。一方、後者では、高周波信号が固定され、磁場強度が徐々に増加します。

最新のパルスフーリエ変換 NMR 装置 (FT-NMR) では、サンプルに一連の短いパルスが照射されている間、磁場は一定に保たれます。パルスは、原子核をより高いエネルギー状態に励起する、ある範囲の無線周波数に分散されるエネルギーの短いバーストです。各原子核がパルス間の間隔または遅延で緩和し、元のスピン状態に戻ると、自由誘導減衰FID と呼ばれる電気インパルスとしてエネルギーが放出されます。次に、FID はフーリエ変換と呼ばれる数学的手法によって周波数対振幅信号に変換され、NMR スペクトルとして解析・記録されます。

NMR 分光計: 概要

NMR分光計は、強力な磁石、高周波送信機、およびサンプルのスペクトルを記録するためのコンピューターコンソールに取り付けられた検出器で構成されています...

Education

JoVE Core

Analytical Chemistry

分析化学

Unit 1

ユニット1

Principles of Nuclear Magnetic Resonance

核磁気共鳴の原理

KEY TERMS AND CONCEPTS

主要な用語と概念

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 field strength is gradually increased.

Modern instruments use pulsed Fourier-transform NMR, or FT-NMR. In this setup, the magnetic field remains constant and the sample receives a series of short pulses. A pulse is a brief burst of energy spread across a range of radio frequencies, and it excites the nuclei to higher energy states.

Between pulses, each nucleus relaxes and returns to its original spin state. As this happens, the energy is released as an electrical impulse called free induction decay, or FID. A Fourier transform converts the FID into a frequency-versus-amplitude signal, which is then recorded as an NMR spectrum.

How NMR Spectrometers Record Signals

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

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-spectrometers-resolution-and-error-correction

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...

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 spectrometers use magnets, radio waves, and Fourier transform to record spectra from samples with NMR-active nuclei.

How NMR Spectrometers Record Signals | JoVE K12

JoVE Core 分析化学 は、複雑な化学原理をアニメーションで視覚化することで、SI 単位から NMR 分光法を含むトピックをよりわかりやすくします。実験を撮影した実写動画では、これらの概念が世界中の研究所でどのように応用されているかを取り上げています。

analytical chemistry

How NMR Spectrometers Record Signals

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