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X-ray Diffraction of Biological Samples01:10

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X-ray diffraction or XRD is an analytical tool that utilizes X-rays to study ordered structures such as crystalline organic and inorganic samples, polycrystalline materials, proteins, carbohydrates, and drugs.
According to Bragg's law, when X-rays strike the sample positioned on a stage, the rays are  scattered by the electron clouds around the sample atoms. The  X-ray diffraction or scattering is caused by constructive interference of the X-ray waves that reflect off the internal...
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In the late 1800s, the revelation that light extended beyond visible wavelengths led to the discovery of X-rays by Wilhelm Roentgen. Recognized as high-energy electromagnetic radiation with short wavelengths, X-rays prompted exploration into their interaction with crystals. Max von Laue proposed in 1912 that the periodic arrangement of atoms, ions, or molecules in crystals would cause them to diffract X-rays, a hypothesis confirmed through experiments with copper sulfate and zinc sulfide...
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Small and Wide Angle X-Ray Scattering Studies of Biological Macromolecules in Solution
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在水性乳液聚合过程中进行时间解析的小角度X射线散射研究

Adam Czajka1, Steven P Armes1

  • 1Department of Chemistry, University of Sheffield, Dainton Building, Brook Hill, Sheffield S3 7HF, United Kingdom.

Journal of the American Chemical Society
|January 14, 2021
PubMed
概括

这项研究使用时间解析小角度X射线散射 (SAXS) 来研究2,2,2-三乙烯甲基酸盐 (TFEMA) 的乳液聚合. 研究人员观察到无表面活性剂和二硫酸盐 (SDS) 配方之间的颗粒形成有明显差异.

科学领域:

  • 聚合物化学
  • 材料科学
  • 物理化学

背景情况:

  • 水性乳液聚合是一种生产聚合物乳的关键工业过程.
  • 了解聚合动力学和粒子形成对于控制材料特性至关重要.
  • 2,2,2-三乙烯甲基酸盐 (TFEMA) 在现场研究中在X射线散射对比方面具有优势.

研究的目的:

  • 通过时间解析小角度X射线散射 (SAXS) 来研究TFEMA的乳液聚合.
  • 在二硫酸盐 (SDS) 存在或不存在的情况下监测颗粒大小演变和聚合动力学.
  • 通过现场SAXS分析阐明水性乳液聚合的机制.

主要方法:

  • 在60°C时对TFEMA进行硫酸盐启动的水性乳液聚合.
  • 使用可动反应细胞进行时间解析小角度X射线散射 (SAXS).
  • 现场动态光散射 (DLS) 和死后SAXS用于颗粒大小分析.
  • H 核磁共振光谱用于转换的确定.
  • 硬球散射模型适用于粒子增长分析.

主要成果:

  • 形成了精确的球形乳,体积平均直径为353 ± 9 nm (无表面活性剂) 和68 ± 4 nm (SDS).

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  • 在分别80分钟和60分钟内,TFEMA转换率达到99% (无表面活性剂) 和93% (SDS).
  • 在现场SAXS确定了SDS存在的聚合过程中的三个主要间隔,与其他方法一致.
  • 在两种配方中,核化发生在大约6分钟内.
  • 结论:

    • 在无表面活性剂和SDS配方之间观察到颗粒大小和聚合动态的显著差异.
    • 在现场SAXS是一个强大的实时监测乳液聚合机制的工具.
    • 这项研究为TFEMA乳液聚合中的表面活性剂的作用提供了宝贵的见解.