一套恒温环境连续式滴定量热装置的建立及其热谱图分析方法的改进

The Construction of a Constant Temperature Environment-Continuous Titration Calorimeter and the Improvement of Thermogram Analysis

根据滴定量热原理,结合国内实际建立了一套恒温环境连续式滴定量热计。经各种物理性能测试表明,仪器运行稳定可靠,灵敏度为9.91×10^(-5)kmm^(-1),经化学标定(HClO_(4)+NaOH)测得△H_(N)^(0)=-13.341±0.0181kcalmol^(-1)。用本仪器测定银(Ⅰ)-吡啶两级配合物的稳定常数和生成焓,结果与文献值吻合。

A constant temperature environment-continuous titration calorimeter has been constructed in our laboratory with the components commercially available on the market. The tenability of this instrument has been tested and its sensitivity determined to be 9.91×10^(-5)kmm^(-1). This calorimeter was chemically calibrated with the neutralization of strong acid and base (HCIO_(4)+ NaOH) and the value of △H_(N)^(0)=-13.341 kcalmol^(-1) was obtained which is quite agreeable with the literature. The results obtained from the measurement of the thermodynamic properties of Ag(Ⅰ)-pyridine complexation reactions conform nicely with those cited in the literiture. The data evaluation procedures have also been improved in the analysis of thermogram.