Testing methods thermal analysis

Spectrophotometry Chromatographic methods Thermal analysis techniques Gas transmission analysis Physical test methods Miscellaneous techniques... 

As the previous sections have shown, there are a large number of low temperature tests in existence. Even when ad hoc bending tests are disregarded, together with the use of the normal range of physical tests, such as tensile modulus and resilience, and the automation of a mechanical test by thermal analysis, there remain several types of specially developed low temperature tests. The various tests do not all have equal relevance to a given product. A test, or tests, should wherever possible, be chosen to provide the information most relevant to the particular application, but for many quality control purposes a test is used simply as a general indication of low temperature behaviour. Whatever the relative merits of the different methods in any situation, the question of correlation between the methods is frequently asked. 

Antioxidants have been shown to improve oxidative stabiHty substantially (36,37). The use of mbber-bound stabilizers to permit concentration of the additive in the mbber phase has been reported (38—40). The partitioning behavior of various conventional stabilizers between the mbber and thermoplastic phases in model ABS systems has been described and shown to correlate with solubiHty parameter values (41). Pigments can adversely affect oxidative stabiHty (32). Test methods for assessing thermal oxidative stabiHty include oxygen absorption (31,32,42), thermal analysis (43,44), oven aging (34,45,46), and chemiluminescence (47,48). 

Assessing the Thermal Stability of Chemicals by Methods of Differential Thermal Analysis, American Society for Testing and Materials, Philadelphia. 

In addition to chemical analysis a number of physical and mechanical properties are employed to determine cemented carbide quaUty. Standard test methods employed by the iadustry for abrasive wear resistance, apparent grain size, apparent porosity, coercive force, compressive strength, density, fracture toughness, hardness, linear thermal expansion, magnetic permeabiUty, microstmcture, Poisson s ratio, transverse mpture strength, and Young s modulus are set forth by ASTM/ANSI and the ISO. 

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). 

Acceptable comprehensive methods of analysis are analytical, model-test, and chart methods, which evaluate for the entire piping system under consideration the forces, moments, and stresses caused by bending and torsion from a simultaneous consideration of terminal and intermediate restraints to thermal expansion and include all external movements transmitted under thermal change to the piping by its terminal and intermediate attachments. Correction factors, as provided by the details of these rules, must be applied for the stress intensification of curved pipe and branch connections and may be applied for the increased flexibihty of such component parts. 

This second group of tests is designed to measure the mechanical response of a substance to applied vibrational loads or strains. Both temperature and frequency can be varied, and thus contribute to the information that these tests can provide. There are a number of such tests, of which the major ones are probably the torsion pendulum and dynamic mechanical thermal analysis (DMTA). The underlying principles of these dynamic tests have been covered earlier. Such tests are used as relatively rapid methods of characterisation and evaluation of viscoelastic polymers, including the measurement of T, the study of the curing characteristics of thermosets, and the study of polymer blends and their compatibility. They can be used in essentially non-destructive modes and, unlike the majority of measurements made in non-dynamic tests, they yield data on continuous properties of polymeric materials, rather than discontinuous ones, as are any of the types of strength which are measured routinely. 

In addition to these standardised test methods set by regulation (in particular the transport regulations of dangerous substances), there are laboratory methods that can provide more details regarding substance behaviour. In particular, there is differential thermal analysis (DTA), thermal gravimetric analysis, calorimetry and thermomanometry, which will not be described here. 

ASTM E 1356-98, ASTM Book of Standards 2002. Standard Test Method for Assignment of the Glass Transition Temperature by Differential Scanning Calorimetry or Differential Thermal Analysis . ASTM International, Conshohocken, PA. 

The presence and concentration of various metallic elements in petroleum coke are major factors in the suitability of the coke for various uses. In the test method (ASTM D5056), a sample of petroleum coke is ashed (thermally decomposed to leave only the ash of the inorganic constituents) at 525°C (977°F). The ash is fused with lithium tetraborate or lithium metaborate. The melt is then dissolved in dilute hydrochloric acid and the resulting solution is analyzed by atomic absorption spectroscopy to determine the metals in the sample. However, spectral interferences may occur when using wavelengths other than those recommended for analysis or when using multielement hollow cathode lamps. 

Many different test methods can be used to study polymers and their physical changes with temperature. These studies are called thermal analysis. Two important types of thermal analysis are called differential scanning calorimetry (DSC) and differential thermal analysis (DTA). DSC is a technique in which heat flow away from a polymer is measured as a function of temperature or time. In DTA the temperature difference between a reference and a sample is measured as a function of temperature or time. A typical DTA curve easily shows both Tg and T . 

Oxidation indices, 656-72 peroxide determination, 762-3 peroxide value, 656, 657-64 colorimetry, 658-61 definition, 657 direct titration, 657 electrochemical methods, 663-4 IR spectrophotometry, 661-3 NIR spectrophotometry, 663 UV-visible spectrophotometry, 658-61 secondary oxidation products, 656, 665-72 tests for stability on storage, 664-5, 672 thermal analysis, 672 Oxidative amperometiy, hydroperoxide determination, 686 Oxidative cleavage alkenes, 1094-5 double bonds, 525-7 Oxidative couphng, hydrogen peroxide determination, 630, 635 Oxidative damage... 

ASTM D 3418-82, Standard Test Method for Transition Temperatures of Polymers by Thermal Analysis, 1982. 

ASTM E831, 2003. Standard test method for linear thermal expansion of solid materials by thermomechanical analysis. 

Thermal and Mechanical Properties of Advanced Heat hield Resinous (CP) and Carbonaceous (CC) Composites, Vol 1. Test Methods, Comparative Data, Recommended Inputs and Analysis , AFML-TR-72-160 Vol-1, Contract F33615-69-C-1796, SRI, Birmingham (1972) 11) J.-P. 

Data reporting (i.e., the statement of the results of the proximate analysis test methods) usually includes (in some countries but not in all countries) descriptions of the color of the ash and of the coke button. As an interesting comparison, the test for determining the carbon residue (Conradson), the coke-forming propensity of petroleum fractions and petroleum products (ASTM D-189 ASTM D-2416), advocates the use of more than one crucible. A porcelain crucible is used to contain the sample, and this is contained within two outer iron crucibles. This corresponds to the thermal decomposition of the sample in a limited supply of air (oxygen) and the measurement of the carbonaceous residue left at the termination of the test. 

Dynamic testing DMTA, DMA, torsional braid analysis (Enns and Gillham, 1983) is first used as a thermal analysis method to detect the transitions, using dissipation peaks. Certain commercial DMTA instruments have a relatively low accuracy in measuring forces and/or strains. In contrast, they give relatively accurate values of the damping factor tan 5, so that dissipation spectra tan 8 = f (oo, T), are very useful analytical tools. 

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