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应用DTA/T/EGD/GC在线联用技术,在空气气氛中对Ge-132的热氧化分解反应历程(室温~925°C)进行了研究,应用X-ray仪对Ge-132在不同温度(450°C、650°C、720°C、800°C、925°C)下的热氧化分解反应残物作了物相鉴定;测定了Ge-132的TG/DTG曲线(室温~970°C);在DTA/T/GC联用曲线的GC谱图上,检出了各反应温度下的O2、CO2和H2O及其热氧化分解产物(逸出气)的组成演变规律。从各残物的XRD谱图上可观察到,Ge-132的晶相结构破坏到720°C时才析出微量Ge、GeO2,并发现Ge在800°C时被氧化为GeO2,至925°C时形成为高纯度GeO2。TGA定量计算表明,Ge-132在空气气氛中被氧化为GeO2的得率与理论计算值相当。综合上述的实验结果与数据分析,对DTA曲线上呈现的二个吸热效应和三个放热效应的性质作出了判断和验证,并得出了Ge-132在空气气氛中被氧化为GeO2的反应历程。
The thermal oxidative decomposition reaction of Ge-132 (room temperature ~ 925 ° C) was carried out in air atmosphere using DTA / T / EGD / GC online technology. (TG) and DTG curves (at room temperature ~ 970 ° C) of Ge-132 were determined by thermal oxidative decomposition reaction at 450 ° C, 650 ° C, 720 ° C, 800 ° C and 925 ° C. The evolution of the composition of O2, CO2 and H2O and their thermal oxidative decomposition products (evolved gas) at each reaction temperature were detected on the GC trace of the DTA / T / GC combination curve. It can be observed from the XRD spectrum of each residue that the Ge-132 crystal phase structure is destroyed to 720 ° C when a small amount of Ge, GeO2 precipitation and found that Ge was oxidized to GeO2 at 800 ° C to 925 ° C When formed as high purity GeO2. Quantitative TGA calculations show that Ge-132 is oxidized to GeO2 in air at a rate comparable to the theoretical value. Based on the above experimental results and data analysis, the properties of two endothermic effects and three exothermic effects on the DTA curve were judged and verified. The results showed that Ge-132 was oxidized to GeO2 in air atmosphere course.