仪器法测定Si-全甲基环硅氮烷的研究

Study on Determining Si-Permethylcyclosilazane by Instrumental Methods

采用~1H NMR、IR和熔点测定法对含八甲基环四硅氮烷(Ⅰ)和六甲基环三硅氮烷(Ⅱ)的固体样品和液体样品进行了定性鉴定。对样品的~1H NMR谱进行了深入解析,纠正了Sadtler标准谱集对NH峰的错误解析。还提出一种以精制的过氧化苯甲酰(BPO)为内标的NMR定量测定方法。用此法获得了Si-甲基环四或环三硅氮烷的纯度、含氮量质量指标及其杂质含量。

Instrumental Methods, namely ~1H NMR, IR and Melting Point Testing, instead of chemical analysis methods are applied for qualitative identification of solid samples containing Si-Octamethylcyclotetrasilazane(Ⅰ) or liquid samples containing Si-Hexamethyleyclotrisilazane(Ⅱ). Investigation resuits of ~1H NMR spectra have corrected a mistaken assignment to NH group in the Sadtler ~1H NMR standard spectra. This paper puts forward a ~1H NMR quantitative determination procedure, in which refined Benzoyl Peroxide (BPO) is employed as an inner standard substance, and specifications of purity of (Ⅰ) and (Ⅱ), Nitrogen-containing ratio and impurity contents in the samples can be calculated from the ~1H NMR spectra.