核磁共振法测定苯基硅橡胶的苯基、乙烯基  

Determination of phenyl and vinyl content in phenyl silicone rubber by nuclear magnetic resonance spectroscopy

作　　者：李辉[1] 孙志勇[1] 李斌[1] 艾惠 邓卫华[1] 杜华太[1] 孙国华[1] 马卫东[1] LI Hui;SUN Zhiyong;LI Bin;AI Hui;DENG Weihua;DU Huatai;SUN Guohua;MA Weidong(Institute 53,China North Industries Group Corporation,Jinan 250031,China;Analytical and Testing Center,Beijing Institute of Technology,Beijing 102400,China)

机构地区：[1]中国兵器工业集团第五三研究所,济南250031 [2]北京理工大学分析测试中心,北京102400

出　　处：《化学分析计量》2019年第4期48-52,共5页Chemical Analysis And Meterage

摘　　要：采用核磁定量技术测定苯基硅橡胶苯基、乙烯基的含量,研究了氘代溶剂种类、脉冲角度、弛豫延迟时间等参数对测定结果的影响。结果表明,氘代氯仿的溶剂峰与苯基共振峰重叠,导致苯基含量测定结果偏高;手动校正谱图相位、基线得到的测定结果波动小;在3~24s范围内,信噪比随着弛豫延迟时间的增加呈下降趋势;信噪比随着采样时间、扫描次数增加而增大。确定的实验条件:溶剂为氘代四氢呋喃,脉冲偏转角为30°,采样次数为128,采样时间为3s,弛豫延迟时间为3s,手动校正谱线。稳定性试验结果的离散系数为0.71%~1.9%(n=5)。用该方法对高纯度甲基苯基环硅氧烷的苯基及甲基乙烯基环硅氧烷中的乙烯基含量进行测试,测定结果分别为100.074%,98.538%,均接近理论值(100%),测定结果的相对标准偏差为0.06%,0.08%(n=5)。该方法稳定性好,精确度良好,可用于苯基硅橡胶苯基、乙烯基含量的测定。The quantitative measurement of phenyl content and vinyl content in phenyl silicone rubber by nuclear magnetic resonance technique was presented. The influence of parameters on the test results and the stability of the test were studied,such as solvent,pulse angle,relaxation pre-delay time and and so on. The results showed that the solvent peak of deuterated chloroform overlaped with the resonance peak of phenyl,which led to the high test result of phenyl content.The measurement results obtained by manually correcting the phase and baseline of spectrogram showed little fluctuation. The ratio of signal to noise decreased with the increasing of the relaxation delay time in the range of 3–24 s. The ratio of signal to noise increased with the increasing of sampling time and scanning times. The experiment conditions were as follows: solvent was deuterated tetrahydrofuran,pulse deflection angle was 30o,sampling times was 128,sampling time was 3 s,relaxation pre-delay time was 3 s,and manual correction spectrogram was used. The dispersion coefficient of stability test results was 0.71%–1.9%(n=5). The results of phenyl content in methyl phenyl cyclosiloxane and vinyl methyl in vinyl cyclosiloxaneby detected by the method were 100.074%,98.538%,respectively,which were close to the theoretical content 100%. The relative standard deviation of detection results were 0.06%,0.08%(n=5),respectively. The method has good stability and accuracy,it is suitable for the determination of phenyl and vinyl content in phenyl silicone rubber.

关 键 词：苯基硅橡胶 苯基 乙烯基 核磁共振法 

分 类 号：O657.2[理学—分析化学]