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相关概念视频

¹H NMR: Complex Splitting01:13

¹H NMR: Complex Splitting

A proton M that is coupled to a proton X results in doublet signals for M. However, NMR-active nuclei can be simultaneously coupled to more than one nonequivalent nucleus. When M is coupled to a second proton A, such as in styrene oxide, each peak in the doublet is split into another doublet.
Splitting diagrams or splitting tree diagrams are routinely used to depict such complex couplings. While drawing splitting diagrams, the splitting with the larger coupling constant is usually applied first.
¹H NMR: Pople Notation01:09

¹H NMR: Pople Notation

The Pople nomenclature system classifies spin systems based on the difference between their chemical shifts. Coupled spins are denoted by capital letters with subscripts indicating the number of equivalent nuclei. When the coupled nuclei have well-separated chemical shifts, they are assigned letters that are far apart in the alphabet, such as A and X. When the difference in chemical shifts is small, coupled nuclei are named using adjacent letters of the alphabet (AB, MN, or XY).
A proton...
¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR01:15

¹H NMR of Conformationally Flexible Molecules: Variable-Temperature NMR

The axial and equatorial protons in cyclohexane can be distinguished by performing a variable-temperature NMR experiment. In this process, except for one proton, the remaining eleven protons are replaced by deuterium. The deuterium substitution avoids the possible peak splitting caused by the spin-spin coupling between the adjacent protons. The remaining proton flips between the axial and equatorial positions.
¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)01:20

¹³C NMR: Distortionless Enhancement by Polarization Transfer (DEPT)

When proton-coupled carbon-13 spectra are simplified by a broadband proton decoupling technique, structural information about the coupled protons is lost. Distortionless enhancement by polarization transfer (DEPT) is a technique that provides information on the number of hydrogens attached to each carbon in a molecule. While the DEPT experiment utilizes complex pulse sequences, the pulse delay and flip angle are specifically manipulated. The resulting signals have different phases depending on...
¹H NMR of Conformationally Flexible Molecules: Temporal Resolution00:52

¹H NMR of Conformationally Flexible Molecules: Temporal Resolution

At room temperature, the chair conformer of cyclohexane undergoes rapid ring flipping between two equivalent chair conformers at a rate of approximately 105 times per second. These two chair conformers are in equilibrium. The rapid ring flipping results in the interconversion of the axial proton to an equatorial proton and an equatorial to the axial proton. Such interconversions are too rapid and cannot be detected on the NMR timescale. Hence, the NMR spectrometer cannot distinguish between the...
Mass Spectrometry of Amines01:15

Mass Spectrometry of Amines

In mass spectroscopy, amines undergo fragmentation to give parent ions with odd molecule weights. This observed mass spectrum follows the nitrogen rule; a molecule with an odd number of nitrogen atoms produces a molecular ion with an odd molecular weight. Amines undergo fragmentation through α cleavage, producing nitrogen-containing cations—iminium ions—and alkyl radicals. Mass spectra of aromatic and cyclic aliphatic amines exhibit strong molecular ion peaks, but acyclic aliphatic amines show...

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MALDI-ToF MS Method for the Characterization of Synthetic Polymers with Varying Dispersity and End Groups
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MALDI-ToF MS Method for the Characterization of Synthetic Polymers with Varying Dispersity and End Groups

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通过使用互补的三甲基末组进行 (1) H NMR 的通用聚合物分析.

Michael Päch1, Daniel Zehm, Maik Lange

  • 1Fraunhofer Institute of Applied Polymer Research, Geiselbergstrasse 69, D-14476 Potsdam-Golm, Germany.

Journal of the American Chemical Society
|June 10, 2010
PubMed
概括

具有三甲基 (TMS) 标记的新型退行链转移剂可使用 (1) H NMR光谱学进行通用聚合物分析. 这些剂提供精确的分子质量和终端组的确定可控的激素聚合,简化聚合物表征.

科学领域:

  • 聚合物化学 聚合物化学
  • 有机合成 有机合成
  • 分析化学 分析化学

背景情况:

  • 控制的激素聚合技术,如可逆添加碎片化链转移 (RAFT) 聚合,对于合成具有定义性质的聚合物至关重要.
  • 准确地描述聚合物分子质量和终端组功能对于理解聚合物的行为和应用至关重要.
  • 传统的分析方法在同时确定这些参数时可能具有挑战性,特别是对于不同的聚合物结构.

研究的目的:

  • 设计和合成用于控制激素聚合的新型退行链转移剂.
  • 通过 (1) H NMR光谱学来证明这些新剂对通用聚合物分析的有用性.
  • 为了能够轻松地确定聚合物的绝对摩尔质量和终端组含量.

主要方法:

  • 设计和合成双重标记的退行链转移剂与补充的三甲基 (TMS) 标记.
  • 这些药物的应用在各种单体 (n-丁烯酸,烯,模拟物) 的可逆添加-碎片化链转移 (RAFT) 聚合过程中.
  • 使用常规的 (1) H NMR光谱学分析得到的聚合物,以确定分子质量和终端组含量.

主要成果:

  • 使用新的RAFT剂获得了具有低多分散度和高摩尔质量的聚合物.
  • 常规的 (1) H NMR 频谱允许准确地确定摩尔质量高达 10~5) g/mol 和终端组含量 (>95%).

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Characterization of Synthetic Polymers via Matrix Assisted Laser Desorption Ionization Time of Flight (MALDI-TOF) Mass Spectrometry
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Characterization of Synthetic Polymers via Matrix Assisted Laser Desorption Ionization Time of Flight (MALDI-TOF) Mass Spectrometry

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Single-throughput Complementary High-resolution Analytical Techniques for Characterizing Complex Natural Organic Matter Mixtures
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Single-throughput Complementary High-resolution Analytical Techniques for Characterizing Complex Natural Organic Matter Mixtures

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MALDI-ToF MS Method for the Characterization of Synthetic Polymers with Varying Dispersity and End Groups
06:16

MALDI-ToF MS Method for the Characterization of Synthetic Polymers with Varying Dispersity and End Groups

Published on: October 3, 2025

Characterization of Synthetic Polymers via Matrix Assisted Laser Desorption Ionization Time of Flight (MALDI-TOF) Mass Spectrometry
06:56

Characterization of Synthetic Polymers via Matrix Assisted Laser Desorption Ionization Time of Flight (MALDI-TOF) Mass Spectrometry

Published on: June 10, 2018

Single-throughput Complementary High-resolution Analytical Techniques for Characterizing Complex Natural Organic Matter Mixtures
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Single-throughput Complementary High-resolution Analytical Techniques for Characterizing Complex Natural Organic Matter Mixtures

Published on: January 7, 2019

  • 补充的TMS终端组标记物揭示了RAFT聚合适性的溶剂依赖差异.
  • 结论:

    • 新开发的RAFT剂是通过 (1) H NMR光谱学进行通用聚合物分析的强大工具.
    • 这些介质有助于确定绝对摩尔质量和终端组含量,这对于合成高质量的聚合物,如远离体和块共聚合物至关重要.
    • 初步结果表明,在类似的原子转移激素聚合 (ATRP) 系统中具有潜在的适用性.