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建立了样品池容积为 7.4cm3 ,可在 70～ 5 80K温区工作的小样品量自动绝热量热计 .量热计设置有两层绝热屏 ,三层辐射屏及辅助控温套 ,以保证高温下量热系统良好的绝热条件 .样品池主体用紫铜制作 ,带有装卸管的容器上盖用黄铜制作 ,紫铜压帽盖与装卸管用螺纹连接铅锡合金垫片密封 ,保证样品池在整个实验温区保持高真空密封不泄漏 .量热计所有导线采用W30 11有机硅耐高温漆绝缘和固定 ,使量热计电测系统在高温下具有良好的稳定性 .所有量热测试数据 ,包括电能和温度的测量 ,全部由计算机按预定程序自动采集和处理 .测量量热标准物质α Al2 O3 的摩尔热容 ,检验了所建量热装置的可靠性 .α Al2 O3 的摩尔热容实验值与舒平值的标准偏差为± 0 .2 8%,与美国标准局数据比较 ,相对偏差在± 0 .4%以内
A small sample volume automatic adiabatic calorimeter with a sample cell volume of 7.4cm3 and working in the temperature range of 70-580K was established.The two-layer adiabatic screen, three-layer radiation screen and auxiliary temperature-controllable thermometer were set in the calorimeter to ensure High temperature calorimetric system good adiabatic conditions.The main body of the sample cell is made of copper, the top of the container with the loading and unloading tube is made of brass, the copper pressure cap and the pipe of the loading and unloading pipe are sealed with the lead-tin alloy gasket, The entire experimental temperature to maintain high vacuum seal does not leak all the thermometers W30 11 silicone high temperature paint insulation and fixed so that the calorimeter electrical measurement system with good stability at high temperatures.All calorimeter test data, Including the measurement of electrical energy and temperature, all by the computer automatically according to a predetermined program to collect and process.Measuring the calorific value of the thermal standard α Al2 O3, test the reliability of the built calorimeter.α molar heat capacity of Al 2 O 3 experiment The standard deviation of value and comfort level was ± 0.28%. Compared with the data of the United States Bureau of Standards, the relative deviation was within ± 0.4%