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Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

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In an NMR sample, precise measurement of the absolute absorption frequencies of nuclei is difficult. A standard internal reference compound is added, and the frequency difference between the reference signal and sample signals is measured.
The internal reference compound generally used in NMR spectroscopy is tetramethylsilane (TMS). TMS is preferred because it is chemically inert, soluble in NMR solvents, and easily removable. Also, the highly shielded methyl protons in TMS yield an intense...
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NMR Spectrometers: Overview01:20

NMR Spectrometers: Overview

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NMR spectrometers consist of a strong magnet, a radiofrequency transmitter, and a detector attached to a computer console for recording spectra of samples containing NMR-active nuclei. In first-generation NMR instruments called continuous-wave spectrometers, the resonance frequencies of the nuclei are determined by frequency-sweep or field-sweep methods. The magnetic field strength is fixed and the rf signal is swept in the former, while the radiofrequency signal is fixed and the magnetic field...
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2D NMR: Overview of Homonuclear Correlation Techniques01:16

2D NMR: Overview of Homonuclear Correlation Techniques

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Homonuclear correlation spectroscopy (COSY) is a powerful technique used in Nuclear Magnetic Resonance (NMR) spectroscopy to study the correlations between nuclei of the same type within a molecule. It provides information about scalar couplings between adjacent nuclei, which helps determine connectivity and structural information. There are several COSY variants, each with its unique strengths and experimental parameters.
COSY90 is the standard two-dimensional (2D) COSY experiment that...
232
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

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Spin systems where the difference in chemical shifts of the coupled nuclei is greater than ten times J are called first-order spin systems. These nuclei are weakly coupled, and their chemical shifts and coupling constant can generally be estimated from the well-separated signals in the spectrum.
As Δν decreases and the signals move closer, the doublets appear increasingly distorted. The intensities of the inner lines increase at the cost of those of the outer lines as the signals are...
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Double Resonance Techniques: Overview01:12

Double Resonance Techniques: Overview

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Double resonance techniques in Nuclear Magnetic Resonance (NMR) spectroscopy involve the simultaneous application of two different frequencies or radiofrequency pulses to manipulate and observe two distinct nuclear spins. One important application of double resonance is spin decoupling, which selectively suppresses coupling with one type of nucleus while observing the NMR signal from another nucleus, simplifying the spectrum and enhancing resolution.
Spin decoupling is usually achieved by...
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NMR Spectroscopy: Spin–Spin Coupling01:08

NMR Spectroscopy: Spin–Spin Coupling

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The spin state of an NMR-active nucleus can have a slight effect on its immediate electronic environment. This effect propagates through the intervening bonds and affects the electronic environments of NMR-active nuclei up to three bonds away; occasionally, even farther. This phenomenon is called spin–spin coupling or J-coupling. Coupling interactions are mutual and result in small changes in the absorption frequencies of both nuclei involved. While nuclei of the same element are involved...
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NMR-Based Fragment Screening in a Minimum Sample but Maximum Automation Mode
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固态NMR中的自动化

Christof Johann1, Sebastian Wegner1, Gerhard Althoff1

  • 1Buker Biospin Rudolf-Plank-Str. 23, 76275 Ettlingen, Germany.

Journal of magnetic resonance (San Diego, Calif. : 1997)
|September 17, 2023
PubMed
概括

在固态NMR (ssNMR) 中自动化射频场设置显著减少了实验时间. 这种方法优化了基于魔法角度旋转 (MAS) 频率的参数,提高了高通量分析的效率.

科学领域:

  • 固态核磁共振 (ssNMR) 光谱学 固态核磁共振 (ssNMR) 光谱学
  • 分析化学 分析化学
  • 频谱学自动化自动化

背景情况:

  • 固态NMR实验需要精确的射频 (rf) 场校准,通常涉及耗时的手动优化.
  • 现有的硬件在某些方面提供了自动化,但实验设置,特别是RF场参数,仍然是一个瓶.
  • 关键的rf场,如旋锁,再合和解是至关重要的,并且通常取决于魔力角旋转 (MAS) 频率.

研究的目的:

  • 开发和验证一种自动化的方法来建立固态NMR实验,重点是射频 (rf) 场参数.
  • 为了减少与传统手动优化RF功率和相关设置相关的时间和复杂性.
  • 通过简化基本ssNMR实验的自动化来实现高通量分析任务.

主要方法:

  • 实施一个在数据采集之前基于实时MAS旋转频率读取所需的RF振幅参数的系统.
  • 使用全局表和脚本自动提供与硬件相关的参数.
  • 开发用于快速MAS实验 (40kHz以上) 的半自动化程序,涉及与MAS频率相对应的哈特曼-哈恩匹配RF场的同步变化.
  • 将自动化方法应用于需要旋转器同步RF场的脱和重新合序列.

主要成果:

  • 实现了基本ssNMR实验的自动设置,消除了在适度的MAS频率上手动优化RF功率的需要.

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  • 证明最佳灵敏度超过理论最大值的90%.
  • 对于快速的MAS交叉极化 (CP) 实验,设置步骤减少了多达一个数量级.
  • 成功地将该方法应用于旋翼同步解和重新合序列.
  • 结论:

    • 提出的方法有效地自动化了固态NMR中关键rf参数的设置.
    • 这种自动化显著提高了效率,减少了实验时间,使得高吞吐量分析成为可能.
    • 该方法简化了复杂的实验,通过将优化重点放在旋转系统属性上,而不是光谱仪硬件调整.