Evaluation of accuracy and reproducibility of a high-temperature differential scanning calorimeter by specific heat and enthalpy of fusion measurements

Author

Susan Jacob

Abstract

"This thesis focuses on developing a set of optimum experimental parameters for high-temperature differential scanning calorimetry. A high-temperature differential scanning calorimeter (HTDSC) was used to check the accuracy and uncertainty of HTDSC measurements upon varying experimental parameters. A set of experimental variables was selected and specific heat or enthalpy of fusion measurements were carried out as case studies. The specific heat of platinum was measured from room temperature to 1400°C by varying heating rate, sample mass, cover gas flow rate, and standard material. Reproducible data were obtained for all the runs except for those made using a thinner platinum sample. Accuracy close to 1% was achieved. Accurate and reproducible heat capacity measurements were given by:
a. higher heating rate
b. standard material of the same size, mass, and geometry that of the sample, and
c. larger sample mass.

For heat of fusion of silver measurements, the type of crucible was also varied to determine its impact on instrument accuracy and reproducibility. Good reproducibility was achieved in the majority of the runs. Accuracy was not satisfactory in most of the runs, though three experimental conditions gave results within 1.7%, 3.3% and 3.5% of the literature value, within the acceptable limits. A larger mass and higher heating rate tended to improve accuracy. Considering the choice of crucibles, alumina-lined platinum crucibles gave better results. Choosing the right experimental conditions and with very careful use, it is possible to obtain accurate and reproducible results using a high-temperature differential scanning calorimeter"--Abstract, page iii.

Advisor(s)

Schlesinger, Mark E.

Committee Member(s)

Fahrenholtz, William
Robertson, D. G. C.

Department(s)

Materials Science and Engineering

Degree Name

M.S. in Materials Science and Engineering

Publisher

University of Missouri--Rolla

Publication Date

Summer 2006

Pagination

viii, 50 pages

Note about bibliography

Includes bibliographical references (pages 47-49).

Rights

© 2006 Susan Jacob, All rights reserved.

Document Type

Thesis - Restricted Access

File Type

text

Language

English

Subject Headings

Calorimeters -- Design and constructionEnthalpy -- MeasurementSpecific heat -- Measurement

Thesis Number

T 8911

Print OCLC #

82453316

Electronic OCLC #

1079419985

Recommended Citation

Jacob, Susan, "Evaluation of accuracy and reproducibility of a high-temperature differential scanning calorimeter by specific heat and enthalpy of fusion measurements" (2006). Masters Theses. 3860.
https://scholarsmine.mst.edu/masters_theses/3860