Differential determined glass transitions

Thermal properties PLA, ionic liquids and their compounds were characterized, a) by differential scanning calorimetry, DSC, (TA Instruments, QA 100 analyzer) from 0°C to 150°Qt a heating rate of 20°lGnin to determine glass transition temperature and b) by thermogravimetric analysis, TGA, (TA Instruments, QA 50 analyzer) from room temperature to 500°C, at a heating rate of 20°C /min in a nitrogen atmosphere to determine thermal stability. 

Glass-transition temperatures are commonly determined by differential scanning calorimetry or dynamic mechanical analysis. Many reported values have been measured by dilatometric methods however, methods based on the torsional pendulum, strain gauge, and refractivity also give results which are ia good agreement. Vicat temperature and britde poiat yield only approximate transition temperature values but are useful because of the simplicity of measurement. The reported T values for a large number of polymers may be found ia References 5, 6, 12, and 13. 

The thermal glass-transition temperatures of poly(vinyl acetal)s can be determined by dynamic mechanical analysis, differential scanning calorimetry, and nmr techniques (31). The thermal glass-transition temperature of poly(vinyl acetal) resins prepared from aliphatic aldehydes can be estimated from empirical relationships such as equation 1 where OH and OAc are the weight percent of vinyl alcohol and vinyl acetate units and C is the number of carbons in the chain derived from the aldehyde. The symbols with subscripts are the corresponding values for a standard (s) resin with known parameters (32). The formula accurately predicts that resin T increases as vinyl alcohol content increases, and decreases as vinyl acetate content and aldehyde carbon chain length increases. 

Differential scanning calorimetry (DSC) is fast, sensitive, simple, and only needs a small amount of a sample, therefore it is widely used to analyze the system. For example, a polyester-based TPU, 892024TPU, made in our lab, was blended with a commercial PVC resin in different ratios. The glass transition temperature (Tg) values of these systems were determined by DSC and the results are shown in Table 1. 

Glass transition temperature (Tg), measured by means of dynamic mechanical analysis (DMA) of E-plastomers has been measured in binary blends of iPP and E-plastomer. These studies indicate some depression in the Tg in the binary, but incompatible, blends compared to the Tg of the corresponding neat E-plastomer. This is attributed to thermally induced internal stress resulting from differential volume contraction of the two phases during cooling from the melt. The temperature dependence of the specific volume of the blend components was determined by PVT measurement of temperatures between 30°C and 270°C and extrapolated to the elastomer Tg at —50°C. 

QO2— ). Glass transition temperatures (Tg s) of copolymers I and IV were determined by the use of a differential scanning calorimeter. The samples were heated at 10 C/minute In air, to 200 C, then cooled and reheated. Glass transition data was taken from the "second heating". 

Thermal Properties. Each of the polyimide film samples was evaluated by differential scanning calorimetry to determine the glass transition temperature (Table I). The general observation is that the BTDA-ODA polyimide films have a higher glass transition temperature than the BDSDA-ODA polyimide films whether they are nonmodifled or are modified with cobalt chloride. This is in agreement with the work of Frye ( ) in which the dianhydride moiety, not the dieunine, was found to control the polyimide glass transition temperature. 

The measurements of Young s modulus in dependence of the temperature (dynamic-mechanical measurements, see Sect. 2.3.5.2) and the differential thermal analysis (DTA or DSC) are the most frequently used methods for determination of the glass transition temperature. In Table 2.10 are listed and values for several amorphous and crystalline polymers. 

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