正辛基二茂铁标准物质的制备及定值

doi:10.11944/j.issn.1000-0518.2018.07.170239

摘要/Abstract

摘要：

烷基取代的二茂铁因其优良的催化性能和制药性能,在国防领域中常被用作固体火箭推进剂的燃速催化剂,而目前正辛基二茂铁没有标准物质,使得相关产品的性能难以得到保证。因此,本研究以工业品正辛基二茂铁为原材料,利用混合溶剂低温重结晶的方法制备了相对纯度大于99.5%的正辛基二茂铁,利用气相色谱法对标准物质候选物进行均匀性和稳定性研究。采用质量平衡法对正辛基二茂铁标准物质定值,主成分自身对照法对其中正辛基二茂铁的同系物杂质进行定值,得到的标准物质纯度为99.6%,对定值结果进行不确定度评估,得到扩展不确定度为0.2%(k=2)。

关键词: 正辛基二茂铁, 标准物质, 质量平衡法, 不确定度

Abstract:

Octylferrocene is often used as a burning rate catalyst for solid rocket propellants because of its excellent catalytic performance and good compatibility. However, so far, there is no its reference material, which makes it difficult to trace and unify the magnitude of the weapons and equipment quality monitoring process, and the quality of related products can not be guaranteed. The reference material of n-octylferrocence in relative purity greater than 99.5% was prepared from industrial product as primary substance by re-crystalization from mixed solvent at low temperature, and its uniformity and stability was investigated by gas chromatography. The purity of n-octylferrocence reference material was certified by the method of mass balance. Other homologues were controlled by self-contrast method. The result shows that the certified result is 99.6% and the expanded uncertainty is 0.2%(k=2).

Key words: n-octylferrocene, certified reference material, mass balance method, uncertainty

田丹,刘强,陈芳,马晓燕. 正辛基二茂铁标准物质的制备及定值[J]. 应用化学, 2018, 35(7): 849-856.

Dan TIAN,Qiang LIU,Fang CHEN,Xiaoyan MA. Preparation and Certification of n-Octylferrocene Certified Reference Material[J]. Chinese Journal of Applied Chemistry, 2018, 35(7): 849-856.

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