波谱学杂志 ›› 1985, Vol. 2 ›› Issue (3): 237-242.

• 研究论文 • 上一篇    下一篇

双共振1H NMR方法测定聚硅氧烷中羟基、乙氧基和乙烯基的含量

石和平   

  1. 晨光化工研究院一分院
  • 收稿日期:1985-03-23 修回日期:1985-05-15 出版日期:1985-09-05 发布日期:2018-01-23

DETERMINATION OF HYDROXYL, ETHOXYL AND VINYL CONTENT OF POLY (DIMETHYL SILOXANES) BY DOUBLE IRRADIATION 1H NMR

Shi Heping   

  1. Chen Guang Research Institute of Chemical Industry
  • Received:1985-03-23 Revised:1985-05-15 Online:1985-09-05 Published:2018-01-23

摘要: 脉冲调制双照射1H NMR方法用来测定聚二甲基硅氧烷中羟基、乙氧基和乙烯基的含量。利用这种方法,仅用了几分钟时间(150次累加)就测定出含量为0.064%的乙烯基。
在本论文中,一共列出了八个样品中各活性基团的测定结果。其相对标准偏差小于5%。
与普通的1H NMR方法相比,该方法可使仪器对聚二甲基硅氧烷中各微量基团的检测极限提高大约1000倍;并且使得采样时间减少几百倍。v2频率的干扰小于0.5ppm并提高了光谱的分辨率。

Abstract: The pulse-modulated double irradiation 1H NMR method is used to determine the content of hydroxyl, ethoxyl and vinyl gruops bonded to the silicon atoms in poly (dimethyl siloxanes). Only in a few minutes (150 times accumulation) the 0.064% vinyl content in the polymer is detected with this method.
In present paper, the determined results of eight samples are illustrated. The relative standard deviations are less than 5%.
As compared with usual method, the limit of instrument detecting active groups of the poly (dimethyl siloxanes) has been increased by about 1000 times and sampling time has also been decreased by several hundred times with this method. The disturbance of v2 frequency is less than 0.5 ppm and the spectra resolutions have been proved.