Introduction to. Thermal Analysis. Techniques and Applications. Second Edition. Michael E. Brown. Kluwer Academic Publishers. Introduction to Thermal Analysis. Techniques and Applications. Edited by. Michael E. Brown. Chemistry Department,. Rhodes University,. Grahamstown, South. to Thermal Analysis Techniques and Applications Edited by Michael E. Brown DRM-free; Included format: PDF; ebooks can be used on all reading devices.
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- Introduction to thermal analysis, Techniques and applications. (Michael E. Brown).pdf - Ebook download as PDF File .pdf) or read book online. 1. INTRODUCTION. The International Confederation of Thermal Analysis and Calorimetry  defines “Thermal Analysis” as a set of techniques. Introduction to Thermal Analysis: Techniques and Applications DOWNLOAD PDF Thermal Analysis: Fundamentals and Applications to Polymer Science.
Purchase Instant Access. View Preview. Learn more Check out. Abstract Thermal analysis includes a number of important techniques which have in common the characterization of materials by describing their properties, or changes in their properties, as a function of temperature and time. Characterization of Materials Browse other articles of this reference work: Related Information.
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In addition to supporting other thermal analysis techniques, TGA is extremely useful in studying various kinetic processes of solids and liquids as long as the processes involve the loss of mass. Other common applications in the pharmaceutical sciences include the characterization of hydrates including the desolvation process and the determination of decomposition, vaporization or sublimation temperatures.
This may be a convenient and time saving feature and although quite accurate, the performance of each technique does suffer somewhat due to construction requirements. Although most thermal analysis methods can deal with samples as solids, semi-solids or liquids, a review of the current literature would suggest that the broad term, solid-state characterization, could apply to a majority of the applications in pharmaceutical research.
Common applications include the characterization of the physicochemical properties of crystalline solids and the detection and identification of polymorphic forms.
With the increased utilization of solid dispersions and other polymeric dosage forms, thermal analytical techniques have been called upon more frequently to aid researchers with their development and characterization. Thermal analytical techniques are also used to study the effects of lyophilization and to develop optimal lyophilization formulations and cycles. Several techniques are also used to study kinetics in the solid-state, including decomposition, accelerated stability and the effects of aging on various formulations.
A crystalline solid may form polymorphs under common manufacturing conditions. Because the physicochemical properties of various polymorphs can vary greatly, identifying the possibility of polymorph formation is critical in product development. DSC has proven to be very useful in the identification of polymorphic transitions primarily due to the ability to easily study the sample under various heating and cooling conditions needed to induce the polymorph formation [7,8,9,10].
Additionally once identified, DSC can be used to monitor samples for the development of polymorphs under various storage conditions or under various manufacturing conditions such as grinding, heating, and drying [11, 12].
Efforts to formulate drugs with poor aqueous solubility and bioavailability have led to the increased utilization of solid dispersions. Solid dispersions consist of at least two solid components one being the matrix forming component the other being the drug.
The drug may be dispersed in the matrix as either crystals, amorphous clusters or uni-molecularly in what is commonly termed a solid solution.
These dispersions may then be formulated into granules, beads, films, microspheres, tablets etc. Karavas, et. DSC revealed that partial miscibility was present between the two components which led to an optimal glass dispersion of the felodipine in the matrix and resulted in a significant enhancement of the dissolution and release kinetics of the felodipine.
Similarly, Mura, et.
DSC was used to characterize and confirm the formation of the dispersions produced by various techniques and dissolution profiles were studied with standard methods.
Solid dispersion formulations are also finding increased use in the development of transdermal formulations. Cho, et. The dispersion, which was also studied by X-ray diffraction, was found to contain quinupramine in an amorphous state which led to enhanced drug release.
DSC results showed that the pure drug existed in the crystalline state and remained in the crystalline state after a physical mixture with EVA was produced as evidenced by an endothermic peak corresponding to the melting point of pure drug. However after a 1: Repka, et. DSC methods were used to assess the miscibility of drug-polymer and polymer-polymer blends and to determine formulations most likely to produce solid solutions or dispersions upon extrusion.
Additionally, samples could be analyzed post extrusion to confirm the solid solution or dispersion formation and periodically sampled form accelerated storage conditions to determine if drug was recrystallizing in the matrix. Another important application was predicting optimal extrusion conditions while using the small sample sizes utilized in DSC.
Thermal analysis DSC and TGA was used to determine temperatures at which drug decomposition occurred and temperatures at which the polymers or polymer blends would melt which is critical in predicting extrusion temperatures that will assure polymer melting yet reduce drug degradation.
Studies could also be performed in which formulations were held isothermally at determined temperatures to study the effects of dwell time in the extruder. Other examples of the complexities encountered when dealing with HME products can be found in recent work published by Qi et.
In this work solid dispersions of paracetamol were prepared in a copolymer based on dimethylaminoethyl methacrylate and neutral methacrylic esters by hot-melt extrusion. A review of this topic is available in American Pharmaceutical Review .
DinNunzio et. PVAP particles displayed positive deviations from expected values suggesting hydrogen bonding between the drug and polymer. Further in vitro and in vivo testing revealed improved bioavailability and enhanced intestinal targeting for the CAP containing particles.
Studies are also available addressing the use of MT-DSC in the analysis of crystal growth from pharmaceutical melts  and pharmaceutical liquid crystals . A review of the recent literature, application notes from manufacturers as well as instrument brochures and websites would certainly confirm this.
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