Authors:S. Cebulak, B. Smieja-Król, S. Duber, M. Misz and A. Morawski
The paper presents the applicability of Oxyreactive Thermal Analysis (OTA) for the investigation of different kinds of carbon
matter. For comparative reasons and more precise interpretation, along with OTA some physico-chemical properties of analyzed
materials were used as the methods commonly applied for the investigations.
The carbon materials of both natural (anthracites, graphite and diamonds) and synthetic origin (active carbon, glass carbon,
expanded graphite, soot and synthetic diamonds) were investigated.
It was stated that there is close relationship between structure parameters and physico-chemical properties and the thermal
reactivity within the investigated groups of carbon matters. The results show that OTA can be accepted as a good investigative
way for such materials.
low temperature formation of crystalline zinc oxide via thermal decomposition
of zinc acetylacetonate monohydrate C10H14O4ZnH2O was studied by humidity controlled thermal analysis. The thermal decomposition
was investigated by sample-controlled thermogravimetry (SCTG), thermogravimety
combined with evolved gas analysis by mass spectrometry (TG-MS) and simultaneous
differential scanning calorimetry and X-ray diffractometry (XRD-DSC). Decomposition
in dry gas by linear heating began with dehydration around 60C, followed
by sublimation and decomposition above 100C. SCTG was useful because
the high-temperature parallel decompositions were inhibited. The decomposition
changed with water vapor in the atmosphere. Formation of ZnO was promoted
by increasing water vapor and could be synthesized at temperatures below 100C.
XRD-DSC equipped with a humidity generator revealed that C10H14O4ZnH2O decomposed directly to the crystalline ZnO by reacting with
This review traces the development of thermal analysis over the last 50 years as it was experienced and contributed to by
the author. The article touches upon the beginning of calorimetry and thermal analysis of polymers, the development of differential
scanning calorimetry (DSC), single-run DSC, and other special instrumentations, up to the recent addition of modulation to
calorimetry and superfast calorimetry.
Many new words and phrases have been introduced to the field by the author and his students, leaving a trail of the varied
interests over 50 years. It began with cold crystallization and more recently the terms oriented, intermediate phase, glass
transitions of crystals, and decoupled chain segments were coined. In-between the following phenomena were named and studied:
extended-chain crystals, irreversible thermodynamics of melting of polymer crystals, zero-entropy-production melting, dynamic
differential thermal analysis (DDTA), the rule of constant increase of Cp per mobile bead within a molecule at the glass transition temperature, superheating of polymer crystals, melting kinetics,
crystallization during polymerization, chin-folding principle, molecular nucleation, rigid amorphous phase, system of classifying
molecules, macroconformations, amorphous defects, rules for the entropy of fusion based on molecular shape and flexibility,
single-molecule single-crystals, systems for classifying phases and mesophases including condis phases, and the globally metastable
semicrystalline polymers with reversible, local subsystems.
The study of soils is very important in the geological and geological engineering researches. A study of ten samples of soils
was carried out by thermal analysis, and X-Ray Fluorescence Spectrometry to understand soil evolution in Angra dos Reis region,
Rio de Janeiro State, Brazil. The sample collection sites were chosen based on geological characteristics, the soil layer
thickness, the soil composition pattern, and whether or not it was moved either by erosion or by gravitational shifts. Because
of the humid tropical climatic condition, natural soils tend to show great thickness of weathered mantles with formation of
saprolites and saprolite soils. Kaolinite is an important secondary mineral which can be formed from many different minerals,
like k-mica and k-feldspar and can be weathered to gibbsite. The results from TG/DTG and DTA indicated which soils had more weathering, and
the same results were obtained by XRF, when silica/aluminum ratios from samples are compared with thermal analysis results.
Recommendations for reporting of thermal analysis data relating to differential thermal analysis, differential scanning calorimetry,
thermogravimetry and thermomechanical analysis were developed some two decades ago. Since that time there have been significant
changes in the techniques, as well as a greater understanding of the effect of experimental variables on the results obtained
from thermonalytical experiments. This paper reports on a preliminary review of the Recommendations by the Task Group established
by the ICTAC Committee on Standardization to undertake their revision. Particular attention has been paid to the properties
of the sample; control of the instrument variables; and the data acquisition and manipulation by computers.