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相关概念视频

Chemical Shift: Internal References and Solvent Effects01:17

Chemical Shift: Internal References and Solvent Effects

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...
¹H NMR: Interpreting Distorted and Overlapping Signals01:02

¹H NMR: Interpreting Distorted and Overlapping Signals

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 slanted or...
Mass Spectrum: Interpretation01:24

Mass Spectrum: Interpretation

An unknown compound can be established by identifying the molecular ion peak in the mass spectrum. The molecular ion peak is often weak or absent due to the predominance of fragmentation in high-energy electron beams. In such cases, a soft-energy electron beam can be used to scan the spectrum to enhance the intensity of the molecular ion peak. Additionally, chemical ionization, field ionization, and desorption ionization spectra are used to obtain a relatively intense molecular ion peak.To...
High-Resolution Mass Spectrometry (HRMS)01:15

High-Resolution Mass Spectrometry (HRMS)

The resolution of a mass spectrometer depends on the efficiency of separating ions with different ion masses. The mass of an atom is approximated to the sum of the masses of protons and neutrons inside, considering the masses of protons and neutrons as equal. However, the masses of the proton (1.6726 × 10−24 g) and neutron (1.6749 × 10−24 g) are not truly equal. There is a minor error in the expression of atomic masses relative to the simplest atom of hydrogen. For example, the mass of helium...
NMR Spectroscopy: Chemical Shift Overview01:15

NMR Spectroscopy: Chemical Shift Overview

The position of the absorption signal of a sample is reported relative to the position of the signal of tetramethylsilane (TMS), which is added as an internal reference while recording spectra. The difference between the absorption frequencies of the sample and TMS (in Hz) is divided by the spectrometer operating frequency (in MHz) to obtain a dimensionless quantity called the chemical shift. It is reported on the δ (delta) scale and expressed in parts per million.
For instance, the proton...
Polymers: Molecular Weight Distribution01:10

Polymers: Molecular Weight Distribution

For any given polymer, the weight average molecular weight (Mw) is higher than, if not equal to, the number average molecular weight (Mn). The only situation in which the weight average molecular weight and the number average molecular weight are equal is when a polymer consists only of chains with equal molecular weight. However, this never happens in a synthetic polymer, since it is difficult to control the polymerization process up to a molecular level with accuracy to a hundred percent.

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相关实验视频

Updated: Jun 24, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
14:55

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

Published on: September 17, 2017

通过内部参考扩散顺序的NMR光谱学 (DOSY) 预测公式重量.

Deyu Li1, Gerald Kagan, Russell Hopson

  • 1Department of Chemistry, Brown University, Providence, Rhode Island 02912, USA.

Journal of the American Chemical Society
|March 28, 2009
PubMed
概括
此摘要是机器生成的。

本研究引入了一种内部参考相关的DOSY方法,用于确定未知分子的配方重量 (FW). 这种实用技术准确地描述了各种溶剂和度中的物种.

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Application and Methodology of the Non-destructive 19F Time-domain NMR Technique to Measure the Content in Fluorine-containing Drug Products
09:24

Application and Methodology of the Non-destructive 19F Time-domain NMR Technique to Measure the Content in Fluorine-containing Drug Products

Published on: August 22, 2017

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Last Updated: Jun 24, 2026

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy
14:55

Atomic Scale Structural Studies of Macromolecular Assemblies by Solid-state Nuclear Magnetic Resonance Spectroscopy

Published on: September 17, 2017

Application and Methodology of the Non-destructive 19F Time-domain NMR Technique to Measure the Content in Fluorine-containing Drug Products
09:24

Application and Methodology of the Non-destructive 19F Time-domain NMR Technique to Measure the Content in Fluorine-containing Drug Products

Published on: August 22, 2017

科学领域:

  • 分析化学 分析化学
  • 物理化学 物理化学
  • 有机化学 有机化学

背景情况:

  • 配方重量 (FW) 对于表征反应性中间体和有机金属复合物至关重要.
  • 精确的FW测定有助于理解组成,聚合和溶解状态.
  • 现有的方法在不同的溶剂和度条件下可能存在局限性.

研究的目的:

  • 开发和验证一个内部参考相关的DOSY方法来计算FW.
  • 评估方法在不同溶剂和度中的准确性和适用性.
  • 为成功实施这种新的表征技术提供指导方针.

主要方法:

  • 使用的扩散有序光谱学 (DOSY) 具有内部参考标准.
  • 使用相关的DOSY来计算未知物种的配方重量 (FW).
  • 研究了溶剂,度和溶液粘度对准确度的影响.

主要成果:

  • 对于小分子 (DIPA) 和有机金属复合物 (聚合物1) 实现了优异的相关性.
  • 证明相对扩散速率与溶液粘度相反相关,与斯托克斯-爱因斯坦方程保持一致.
  • 发现预测准确度 (r^2,%差异) 与密度变化有关,随着密度的下降而改善.

结论:

  • 内部参考相关的DOSY方法为FW确定提供了实用和准确的方法.
  • 该方法具有多功能性,适用于不同溶液条件下的各种分子和复合物.
  • 这种技术为表征未知的化学物种提供了有价值的工具.