裂解气相色谱法测定含能材料中氟橡胶

Determination of Fluoro-Rubber in Energetic Materials by Pyrolytic Gas Chromatography

应用裂解气相色谱法测定了含能材料中氟橡胶的含量,方法中选用液体进样法,将试样(如聚黑-14及黑索今等样品,以及氟橡胶标准样品)溶解于乙酸乙酯中,分取其中1μL滴于热带探头的铂金带上,经红外灯烘干除去乙酸乙酯后引入于裂解器中,在600℃裂解8s,最适宜的进样量为108μg。在最佳测定条件下,测得的峰高值与氟橡胶的质量浓度在19.2～28.8g·L^(-1)范围内呈线性关系。对方法的精密度进行了试验,测得相对标准偏差(n=11)为0.13%。

Pyrolytic gas chromatography was applied to the determination of fluororubber in energetic materials. Sample introduction in liquid state was preferred in this method. The samples （i. e. the JH-14 the RDX and the fluororubber standard） were dissolved in ethylacetate and an aliquot of 1μL was dropped on the platinum belt of the probe and after drying by a IR-lamp to expel the ethyl acetate, the sample on the platinum belt was introduced into the pyrolyzer, and pyrolyzed at 600 ℃ for 8 s. The optimum quantity of sample introduced was 108μg. Under optimum condition of determination. Linear relationship between values of peak heights and concentration of fluororubber was obtained in the range of 19. 2-28. 8 g ·L^-1. Value of RSD＇s （n= 11） obtained in the precision test was 0. 13%.