Calorimetric Determination of Purity: Design and Operation of a Small Adiabatic Calorimeter
Calorimetric Determination of Purity: Design and Operation of a Small Adiabatic Calorimeter
复制标题
纯度的量热测定：小型绝热量热计的设计和操作
DOI：
10.1021/ac60097a022
复制
发表时间：
1955
影响因子：
7.4
通讯作者：
H. Stone
中科院分区：
文献类型：
--
作者：
D. D. Tunnicliff;H. Stone
研制了一种绝热量热计，用于测定光谱研究所需的参比化合物的纯度。两个可互换的热量计，体积分别为0.5和5ml。一个完整的测定，包括计算，通常需要不到4小时。虽然纯度的测定是基于熔点下降的测量，但与传统的熔点方法不同，这种方法不需要事先测定纯化合物的熔点和熔点。相反，该方法确定这些数量作为分析的一部分。量热计用于测量样品从固态到液态时热量输入的平衡温度。对数据的分析给出了熔合热、样品的熔点和纯化合物的熔点。对于纯度在99.8摩尔%以上的样品，其纯度测定误差小于0.05摩尔%。对于较少杂质的样品，误差随杂质量的增加而增加。
An adiabatic calorimeter has been developed for determination of the purity of the reference compounds re-quired for spectroscopic investigations. Two inter-changeable calorimeterswith volumes of 0.5 and 5 ml. are used. A complete determination, including cal-culations, usually requires less than 4 hours. Although the purity determination is based on the measurement of the melting point depression, this method, unlike conventional melting point methods, does not require a previous determination of the heat of fusion and the melting point of the pure compound. Instead, the method determines these quantities as part of the analysis. The calorimeter is used to measure the equilibrium temperature of the sample as a function of heat input as it passes from the solid state to the liquid state. Analysis of the data gives the heat of fusion, the melting point of the sample, and the melting point of the pure compound. The error in the determination of the purity of samples with a purity above 99.8 mole% is less than 0.05 mole%. For lesspure samples the error increases with the amount of impurity.