GAP相对分子质量标准物质制备及定值与验证研究

Preparation,definite value and verification of molecularweight standard reference material of GAP

为快捷制备聚叠氮缩水甘油醚(GAP)相对分子质量标准物质,在GAP可控聚合基础上开展了逐级沉淀分级法制备与GPC-MALLS法定值研究,并采用13 C-NMR法、粘度法与元素分析法对定值结果进行了验证。结果表明,采用GPC-MALLS法定值,13 C-NMR法等验证的方法可进行GAP相对分子质量标准物质的准确定值。五个级分样品的数均相对分子质量(M n)定值分别为986.5、1569、2041.5、2569.5、3100.5,均相应位于1000±200、1500±200、2000±200、2500±200、3000±200的区间内;分布指数(D)定值分别为1.123、1.146、1.149、1.134、1.162,均小于等于1.2;含氮量分别为38.49%、39.87%、40.43%、40.90%、41.13%,均与相应理论值较为吻合。研究表明,采用阳离子可控聚合技术与逐级沉淀法分级技术相结合的方法可为GAP等含能聚醚粘合剂相对分子质量标准物质研制提供一种快捷简便的方法。

In order to prepare molecular weight standard substance of glycidyl azide polymer(GAP)efficiently,the step-by-step precipitation grating and gel permeation chromatography-laser light scatting(GPC-MALLS)certification of GAP were studied on the basis of GAP controllable polymerization.The results of definite value were verified by 13 C-NMR,viscometry and elemental analysis,respectively.Results show that the accurate definite value of GAP could be obtained by GPC-MALLS and verified by 13 C-NMR.The number-average molecular weights(M n)of five molecular weight grades of standard substance of GAP are 986.5,1569,2041.5,2569.5 and 3100.5,which are respectively located at 1000±200,1500±200,2000±200,2500±200 and 3000±200.The molecular weight dispersion indexes(D)are respectively 1.123,1.146,1.149,1.134 and 1.162,which are less than 1.2.The nitrogen contents are respectively 38.49%,39.87%,40.43%,40.90%and 41.13%,which are in keeping with the theoretical value.The results show that the combination of cationic controlled polymerization technology and stepwise precipitation classification technology can provide a quick and simple method for the preparation of GAP and other energetic polyether binder relative molecular weight reference materials.