摘要
为获得准确可靠的复合推进剂凝聚相燃烧产物(CCPs)的理化特性,提出了一种基于微波消解的乙二胺四乙酸(EDTA)滴定法以实现凝聚相燃烧产物全组分定量解析。采用自研凝聚相燃烧产物收集系统获取了四组元推进剂凝聚相燃烧产物,针对活性Al含量对比分析了EDTA滴定法、电感耦合高频等离子体发射光谱法(ICP)、气体容量法及重铬酸钾滴定法等4种方法的测试精度。结果表明,基于微波消解的EDTA滴定法能准确测定复合推进剂凝聚相燃烧产物中的Al、Al2O3、AlN、Fe2O3和C等组分含量。微波消解能有效溶解包裹在活性Al表面的Al2O3壳层,其最优溶液配比参数为VH3PO4∶VH2SO4∶VHNO3=10∶2∶1,温度为240℃,时间为150 min。ICP光谱法也能检测凝聚相燃烧产物中的全部组分,精度略低于EDTA滴定法。气体容量法和重铬酸钾滴定法测定凝聚相燃烧产物中活性Al的含量则显著低于EDTA滴定法和ICP光谱法。EDTA滴定法测定活性Al含量最精确,其精度相较气体容量法、重铬酸钾滴定法、ICP光谱法分别提高60%,40%,22%。
In order to obtain accurate and reliable physicochemical properties of condensed phase combustion products(CCPs)of composite propellants,a method of ethylenediamine tetraacetic acid(EDTA)titration based on microwave digestion was pro⁃posed to achieve the quantitative analysis of the total components of condensed phase combustion products.Four groups of con⁃densed phase combustion products of propellant were obtained by using self⁃developed condensed phase combustion products collection system.The determination accuracy of EDTA titration,inductively coupled high frequency plasma emission spectrom⁃etry(ICP),gas volumetric method and potassium dichromate titration were compared and analyzed for the content of active Al.The results show that the EDTA titration method based on microwave digestion can accurately determine the contents of Al,Al2O3,AlN,Fe2O3 and C in the condensed phase combustion products of composite propellants.Microwave digestion can effec⁃tively dissolve the Al2O3 shell coating on the surface of active Al.The optimal parameters of microwave digestion is supposed to be VH3PO4∶VH2SO4∶VHNO3=10∶2∶1.The temperature was 240℃,and the digestion time was 150 min.ICP spectroscopy can also de⁃tect all component contents of condensed combustion products,with a precision slightly lower than EDTA titration.The content of active Al in condensed phase combustion products determined by gas volumetric method and potassium dichromate titration was significantly lower than that determined by EDTA titration and ICP spectrometric method.EDTA titration is the most accurate method to determine the content of active Al.Compared with gas volumetric method,potassium dichromate titration method and ICP spectrometric method,the accuracy of EDTA titration is improved by 60%,40%and 22%,respectively.
作者
刘欢
敖文
刘林林
刘露
苟东亮
刘佩进
胡松启
LIU Huan;AO Wen;LIU Lin-lin;LIU Lu;GOU Dong-liang;LIU Pei-jin;HU Song-qi(Science and Technology on Combustion,Internal Flow and Thermo‑Structure Laboratory,Northwestern Polytechnical University,Xi′an 710072,China)
出处
《含能材料》
EI
CAS
CSCD
北大核心
2021年第7期599-606,共8页
Chinese Journal of Energetic Materials
基金
中央高校基本科研业务费专项资金资助(3102018ZY003)。
关键词
复合推进剂凝聚相燃烧产物(CCPs)
成分
微波消解
EDTA滴定法
composite propellant condensed phase combustion products(CCPs)
ingredients
microwave digestion
EDTA titra⁃tion method
