摘要
采用水解缩合法合成了苯基硅油,并进行傅立叶红外(FTIR)、氢谱(1H NMR)表征。根据氢谱的积分,计算得产品的苯基含量。基于苯基基团在紫外区的特征吸收,以自制苯基硅油为标准品,建立了一种紫外分光光度法测定苯基硅油中苯基含量的方法。以二氯甲烷为溶剂,264nm为最大吸收波长,苯基浓度在0.277×10-3～2.13×10-3 mmol.mL-1范围内,符合比尔定律,其R2=0.99946。实际样品测定的相对标准偏差小于1.81%,平均回收率为99.0%左右。该方法线性相关性好、精密度及准确度高、便捷、成本低,适合科研及工业生产中苯基含量的日常分析。
The phenyl silicone oil was prepared by means of hydrolysis-condensation and characterized by FT-IR and 1H NMR.Its phenyl content was obtained according to 1H NMR integral value.Then UV spectrophotometry was employed for the determination of phenyl content in phenyl silicone oil based on the UV absorption of phenyl group.The detection wavelength was 264 nm and dichloromethane was chosen as solvent.The Bill＇s law was obeyed in the range of phenyl concentration of 0.277×10-3 ~2.13×10-3 mmol·mL-1 with R2 of 0.99946.The average recovery for the two spiked samples was about 99.0% and RSD was less then 1.81%.The developed method was low-cost,simple,sensitive,accurate,and is suitable for the routine analysis.
出处
《分析科学学报》
CAS
CSCD
北大核心
2012年第1期79-82,共4页
Journal of Analytical Science
基金
国家自然科学基金(No.20971058)
佛山市产学研专项项目(No.2010B1028)
关键词
紫外分光度法
苯基硅油
苯基含量
UV spectrophotometry
Phenyl silicone oil
Phenyl content
