Differential scanning calorimetry development

Thermal analysis iavolves techniques ia which a physical property of a material is measured agaiast temperature at the same time the material is exposed to a coatroUed temperature program. A wide range of thermal analysis techniques have been developed siace the commercial development of automated thermal equipment as Hsted ia Table 1. Of these the best known and most often used for polymers are thermogravimetry (tg), differential thermal analysis (dta), differential scanning calorimetry (dsc), and dynamic mechanical analysis (dma). 

The worst hazard scenarios (excessive temperature and pressure rise accompanied by emission of toxic substances) must be worked out based upon calorimetric measurements (e.g. means to reduce hazards by using the inherent safety concept or Differential Scanning Calorimetry, DSC) and protection measures must be considered. If handling hazardous materials is considered too risky, procedures for generation of the hazardous reactants in situ in the reactor might be developed. Micro-reactor technology could also be an option. Completeness of the data on flammability, explosivity, (auto)ignition, static electricity, safe levels of exposure, environmental protection, transportation, etc. must be checked. Incompatibility of materials to be treated in a plant must be determined. 

X-ray diffraction studies are usually carried out at room temperature under ambient conditions. It is possible, however, to perform variable-temperature XPD, wherein powder patterns are obtained while the sample is heated or cooled. Such studies are invaluable for identifying thermally induced or subambient phase transitions. Variable-temperature XPD was used to study the solid state properties of lactose [20], Fawcett et al. have developed an instrument that permits simultaneous XPD and differential scanning calorimetry on the same sample [21], The instrument was used to characterize a compound that was capable of existing in two polymorphic forms, whose melting points were 146°C (form II) and 150°C (form I). Form II was heated, and x-ray powder patterns were obtained at room temperature, at 145°C (form II had just started to melt), and at 148°C (Fig. 2 one characteristic peak each of form I and form II are identified). The x-ray pattern obtained at 148°C revealed melting of form II but partial recrystallization of form I. When the sample was cooled to 110°C and reheated to 146°C, only crystalline form I was observed. Through these experiments, the authors established that melting of form II was accompanied by recrystallization of form I. 

Levine and Slade [1.16] investigated the mechanics of cryostability by carbohydrates. Figure 1.19.1 shows an idealized phase diagram developed from differential scanning calorimetry (DSC) measurements for hydrolyzed starch (MW > 100) and for polyhydroxy combinations having a small molecular mass. With slow cooling (quasi in equilibrium conditions), no water crystallizes below the Tg curve. 

Hatley, R. H. M. The effective use of differential scanning calorimetry in the optimisation of freeze-drying processes and formulations. Developments in Biological Standardization Vol. 74, p. 105-122. Acting Editors Joan C. May, F. Brown S. Karger AG, CH-4009 Basel (Switzerland), 1992... 

Development stage, life cycle issues, 20-23 Deviations, risk assessment, 94-95 Differential scanning calorimetry, chemical reactivity tests, 87... 

Source Data from Remmele, R.L., Jr., N.S. Nightlinger, S. Srinivasan, and W.R. Gombotz. 1998. Interleukin-1 receptor (IL-1R) liquid formulation development using differential scanning calorimetry. Pharm Res 15 200-208. 

In recent years, a new research method was developed to determine total starch content of potato dry matter by comparing the gelatinization enthalpy of potato dry matter and standard starch using differential scanning calorimetry (DSC) (Liu et al., 2005). 

The purpose of the second dwell is to allow crosslinking of the matrix to take place. It is during the second dwell when the strength and related mechanical properties of the composite are developed. To characterize the exothermic crosslinking reaction of a thermosetting polymer matrix, a thermal cure monitor technique such as Differential Scanning Calorimetry... 

Thermal analysis is a term used to cover a group of techniques in which a physical property of a substance and/or its reaction product(s) is measured as a function of temperature. This experiment is confined to the area of differential thermal analysis (DTA) and, more specifically, its quantitative development, differential scanning calorimetry (DSC) [1-15]. 

Temperature-rising elution fractionation (tref) is a technique for obtaining fractions based on short-chain branch content versus molecular weight (96). On account of the more than four days of sample preparation required, stepwise isothermal segregation (97) and solvated thermal analysis fractionation (98) techniques using variations of differential scanning calorimetry (dsc) techniques have been developed. 

Interest in the use of calorimetry as a routine diagnostic or analysis tool has gained significant momentum only in the last 50 years. This interest has lead to the development of popular procedures such as differential thermal analysis (DTA) and differential scanning calorimetry (DSC). A wide variety of solution calorimetric techniques exist today. These techniques include thermometric titration, injection and flow emhalpimetry. The major growth of commercial instrumentation for calorimetry has occurred to address applications in routine analysis and the rapid characLerizaiion of materials. 

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