Differential thermal analysis determinations

The glass-tiansition tempeiatuiesfoi solution-polymeiized SBR as well as ESBR aie loutinely determined by nuclear magnetic resonance (nmr), differential thermal analysis (dta), or differential scanning calorimetry (dsc). 

Thermal Properties. The thermal stabiUty of cellulose esters is deterrnined by heating a known amount of ester in a test tube at a specific temperature a specified length of time, after which the sample is dissolved in a given amount of solvent and its intrinsic viscosity and solution color are deterrnined. Solution color is deterrnined spectroscopically and is compared to platinum—cobalt standards. Differential thermal analysis (dta) has also been reported as a method for determining the relative heat stabiUty of cellulose esters (127). 

A variety of instmmental techniques may be used to determine mineral content. Typically the coal sample is prepared by low temperature ashing to remove the organic material. Then one or more of the techniques of x-ray diffraction, infrared spectroscopy, differential thermal analysis, electron microscopy, and petrographic analysis may be employed (7). 

Order of thermal stabiUty as determined by differential thermal analysis is sebacic (330°C) > a2elaic = pimelic (320°C) > suberic = adipic = glutaric (290°C) > succinic (255°C) > oxahc (200°C) > malonic (185°C) (19). This order is somewhat different than that in Table 2, and is the result of differences in test conditions. The energy of activation for decarboxylation has been estimated to be 251 kj/mol (60 kcal/mol) for higher members of the series and 126 kJ/mol (30 kcal/mol) for malonic acid (1). 

Dynamic differential thermal analysis is used to measure the phase transitions of the polymer. IR is used to determine the degree of unsaturation in the polymer. Monitoring of the purity and raw is done commercially using gas phase chromatography for fractionization and R1 with UV absorption at 260 nanometers for polystyrene identification and measurement Polystyrene is one of the most widely used plastics because of fabrication ease and the wide spectrum of properties possible. Industries using styrene-based plastics are packaging, appliance, construction, automotive, radio and television, furniture, toy, houseware and baggage. Styrene is also used by the military as a binder in expls and rocket propints... 

The techniques referred to above (Sects. 1—3) may be operated for a sample heated in a constant temperature environment or under conditions of programmed temperature change. Very similar equipment can often be used differences normally reside in the temperature control of the reactant cell. Non-isothermal measurements of mass loss are termed thermogravimetry (TG), absorption or evolution of heat is differential scanning calorimetry (DSC), and measurement of the temperature difference between the sample and an inert reference substance is termed differential thermal analysis (DTA). These techniques can be used singly [33,76,174] or in combination and may include provision for EGA. Applications of non-isothermal measurements have ranged from the rapid qualitative estimation of reaction temperature to the quantitative determination of kinetic parameters [175—177]. The evaluation of kinetic parameters from non-isothermal data is dealt with in detail in Chap. 3.6. 

The Sr-Cu system has been critically assessed. The most recent phase diagram, determined by combining differential thermal analysis and x-ray diffraction techniques, contains two intermediate compounds, both of which form in peritectic reactions, SrCu (588°C) and SrCu, (845°C) SrCu has also been prepared for independent structural analysis-. ... 

Phase diagrams give valuable information about the compounds that can form in a system of components. These compounds can then be prepared and studied. For the experimental determination of phase diagrams the following methods are used. In differential thermal analysis (DTA) a sample of a given composition is heated or cooled slowly... 

Tang, W. K., H. W. Eickner. Effect of Inorganic Salts on Pyrolysis of Wood, Cellulose, and Lignin Determined by Differential Thermal Analysis FPL Research Paper 82, U.S.D.A., 1967. 

Duckworth, R. B. Differential thermal analysis of frozen food systems. I. The determination of unfreezable water. Joum. Food Technol. 6, p. 317-327, 1971... 

These parameters need to be considered for reactions that go towards the intended completion as well as for possible upsets (see section C). Measuring methodologies for determining characteristic material property values (Stoffkenngrofcen), e.g., differential thermal analysis ("DTA"), calorimetry, and adiabatic experiments, and their possible use and applications are given in the literature /1, 2, 3, 41. 

David, D.J. Determination of specific heat and heat of fusion by differential thermal analysis. Study of theory and operating parameters, Aural Chem., 36(11) 2162-2166, 1964. 

The second section will concentrate on methods of determining phase diagrams. The first part will examine non-isothermal methods, such as differential thermal analysis and cooling curve determinations, while the second will concentrate on isothermal methods, such as metallography, X-ray measurements, etc. The various limitations of both methods will be discussed and some novel techniques introduced. 

More advanced techniques are now available and section 4.2.1.2 described differential scanning calorimetry (DSC) and differential thermal analysis (DTA). DTA, in particular, is widely used for determination of liquidus and solidus points and an excellent case of its application is in the In-Pb system studied by Evans and Prince (1978) who used a DTA technique after Smith (1940). In this method the rate of heat transfer between specimen and furnace is maintained at a constant value and cooling curves determined during solidification. During the solidification process itself cooling rates of the order of 1.25°C min" were used. This particular paper is of great interest in that it shows a very precise determination of the liquidus, but clearly demonstrates the problems associated widi determining solidus temperatures. 

A variety of techniques have been used to determine the extent of crystallinity in a polymer, including X-ray diffraction, density, IR, NMR, and heat of fusion [Sperling, 2001 Wunderlich, 1973], X-ray diffraction is the most direct method but requires the somewhat difficult separation of the crystalline and amorphous scattering envelops. The other methods are indirect methods but are easier to use since one need not be an expert in the field as with X-ray diffraction. Heat of fusion is probably the most often used method since reliable thermal analysis instruments are commercially available and easy to use [Bershtein and Egorov, 1994 Wendlandt, 1986], The difficulty in using thermal analysis (differential scanning calorimetry and differential thermal analysis) or any of the indirect methods is the uncertainty in the values of the quantity measured (e.g., the heat of fusion per gram of sample or density) for 0 and 100% crystalline samples since such samples seldom exist. The best technique is to calibrate the method with samples whose crystallinites have been determined by X-ray diffraction. 

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. 

Differential thermal analysis (DTA) has provided a wealth of information regarding the thermal behavior of pure solids as well as solid mixtures [10]. Melting points, boiling points, transitions from one crystalline form to another, and decomposition temperatures can be obtained for pure materials. Reaction temperatures can be determined for mixtures, such as ignition temperatures for pyrotechnic and explosive compositions. 

Ignition temperatures can also be determined by differential thermal analysis (DTA), and these values usually correspond well to those obtained by a Henkin-McGill study. Differences in heating rate can cause some variation in values obtained with this technique. For any direct comparison of ignition temperatures, it is best to run all of the mixtures of interest under identical experimental conditions, thereby minimizing the number of variables. 

The temperature of maximum transformation rate is easily determined using either of two similar techniques called differential scanning calorimetry (DSC) or differential thermal analysis (DTA). These techniques are extremely useful in the kinetic study of both isothermal and nonisothermal phase transformations. 

There are two types of stages for dynamic microscopy (a) hot and cold stages and (b) tensile stages [1], Hot stages are most commonly used for the dynamic microscopy of polymers [1,43]. Thermal analysis in the OM is complementary to other thermal analysis methods, such as differential thermal analysis (DTA) [1], Direct observation of the structural changes of a polymer as a function of temperature can determine the nature of phase changes and thermal decomposition [1], It also measures the transformation temperatures. 

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