SEDL / STP / STP838-EB / STP32590S

Optimization of Accuracy and Precision in the Differential Scanning Calorimetry Dynamic Purity Method

Hunter, JE
Chemist and supervisor, E. I. du Pont de Nemours & Co., Wilmington, DE

Blaine, RL
Chemist and supervisor, E. I. du Pont de Nemours & Co., Wilmington, DE

Pages: 10    Published: Jan 1984

Download this paper for $25 PDF (136K)          View License Agreement
Abstract

The effects were examined of specimen size, heating rate, impurity level and data acquisition rate on the precision and accuracy of the dynamic purity method employing differential scanning calorimetry. A set of experimental conditions exist which optimize precision and accuracy. These include: (1) specimen size of 1.7 mg, (2) heating rate of 0.5°C/min, (3) impurity level less than 2 mol %, and (4) data acquisition rate of 120 data points/°C. Slight variations from these values may be permitted thus confirming guideline previously reported in the literature. The errors caused by deviations from these values are shown to be cumulative. Thus, if any one of these parameters must deviate from its optimum value, the others should maintain those values to obtain accurate results.