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CONSTRUCTION AND OPERATION PRINCIPLE OF A BLOCK CALORIMETER FOR DETERMINING THE STANDARD ENTHALPIES OF SOLID STATE REACTIONS
Thermochimica Acta ( IF 3.1 ) Pub Date : 2020-09-01 , DOI: 10.1016/j.tca.2020.178706
Е. Osadchii , N. Zhdanov , T. Stolyarova , Е. Brichkina

Abstract The paper describes the design and operation principle of a massive block calorimeter with a vacuum shell and a water thermostat. The calorimeter is designed for determining the enthalpy of solid-state reactions under standard conditions (p = 105 Pa, T = 298.15 K) with metals, chalcogens and chalcogenides with the exception of reactions involving elemental sulfur. The measurement method is based on comparing the amount of heat (the work of an electric current) set for the reaction under study and the amount of heat generated or absorbed during the reaction, measured during the cooling of the system to the standard temperature. The optimal amount of the reagent mixture (1.5 -2.5 g) is placed in a quartz glass ampoule which is then evacuated and sealed. The duration of the main period (heating) is 6-10 minutes and the total experiment time is 50-60 minutes. The maximum heating temperature of the sample is 1273 K. The process of determining the standard enthalpy of a solid-state reaction was studied on the example of Sb2Se3(cr) production from the elements: ΔfH0Sb2Se3 = -(127.91 ± 2.08) kJ / mol.

中文翻译:

测定固态反应标准焓的块式热量计的构造和操作原理

摘要 介绍了真空壳和水温控器块体量热仪的设计和工作原理。该量热仪设计用于在标准条件 (p = 105 Pa, T = 298.15 K) 下测定与金属、硫属元素和硫属元素化物的固态反应焓,但涉及元素硫的反应除外。测量方法基于比较为所研究的反应设定的热量(电流的功)与反应过程中产生或吸收的热量,在系统冷却至标准温度期间测量。将最佳量的试剂混合物 (1.5 -2.5 g) 置于石英玻璃安瓿中,然后将其抽真空并密封。主要阶段(加热)持续时间为6-10分钟,总实验时间为50-60分钟。样品的最高加热温度为1273 K。 以元素生成Sb2Se3(cr)为例研究了固态反应标准焓的测定过程:ΔfH0Sb2Se3 = -(127.91±2.08) kJ/mol .
更新日期:2020-09-01
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