Simultaneous thermal analysis STA

STA (simultaneous thermal analysis) DSC measurements performed on one arm of a thermal balance, thus avoiding ambiguities of sample temperature for combined DSC-TGA. Characterising minor volatile loss and reaction energies. Heats of desorption. 

Simultaneous Thermal Analysis (STA) A technique which combines DTA, TGA, DSC (cal.) and derivatives of DTA/TGA in a single instrument, offers advantages over the performance of each technique as a separate experiment on stand-alone instruments. By examining a single sample, one ensures no variation in sample homogeneity, atmosphere difference and other instrumental parameters. At the same time, there is a provision for detection and analysis of evolved gases (EGA) during thermal decomposition. Also, derivatives of TGA and DTA can be precisely measured (electronically). 

A popular and useful device is a combined DTA/TG (simultaneous thermal analysis STA) system in which both thermal and mass change effects are measured concurrently on the same sample. An example STA study comprising DTA, TG, and DTG for the decomposition of calcium oxalate is shown in Figure 5.7. 

The experiments were carried out in a Netzsch STA 409 C (Simultaneous Thermal Analysis - STA) in the TGA/DSC configuration. The STA has a vertical san le carrier with a reference and a sample crucible, and in order to account for buoyancy effects, a correction curve with empty crucibles was first conducted and then subtracted from the actual experiments. Platinum/Rhodium crucibles were used in order to get the best possible heat transfer. The thermocouple for each crucible was positioned Just below and in contact with the crucible. The ten rerature obtained from the measurement is the temperature in the reference side. This temperature is converted to the temperature in the sample side by using the DSC-signal in pV and a temperature-voltage table for the thermocouple. The product gases were swept away by lOO Nml/inin nitrogen which exited the top of the STA, The STA was calibrated for temperature and sensitivity (DSC) with metal standards at each heating rate. 

This chapter is concerned with the large family of Simultaneous Thermal Analysis (STA) techniques, in which two or more types of measurement are made at the same time on a single sample. This methodology, entailing a more complex instrument, often specially built, has been found to be essential in a variety of thermal studies, and instruments for simultaneous measurements have been constructed for more than fifty years - often as soon as it was technically possible, as the benefits of this approach were rapidly appreciated. 

Simultaneous Thermal Analysis (STA) and Mass Spectrometry Systems) The Fine Work Co. Ltd... 

Some commercial instruments have been developed which combine a thermobalance with a thermal analyzer in a single heating process, recording TG, DTG, and DTA curves simultaneously. Representatives of this kind of equipment are the De-rivatograph (Hungarian Optical Works) shown in Figure 3.7 and the STA system (simultaneous thermal analysis system) of Stanton Redcroft Ltd. (UK). 

While TGA provides useful data when a mass change is involved in a reaction, we have seen that many reactions do not have a change in mass associated with them. The use of both TGA and DTA or TGA and DSC provides much more information about a sample than either technique alone provides. There are several commercial thermal analysis instrument manufacturers who offer simultaneous combination systems, often called simultaneous thermal analysis (STA) systems. Simultaneous TGA-DTA and simultaneous TGA-DSC instruments are available. Instrument combinations cover a wide temperature range and come in both analytical sample size (1-20 mg)... 

Thermo gravimetry (TG) Differential Scatming Calorimetry (DSC) Mass change study. Stmfy of heat difference Simultaneous thermal analysis (STA) [(TG)-K DSC)]... 

The extent of dehydration during temperature treatment of tin(IV)oxide powder is Mcertained by thermogravimetry (Simultaneous Thermal Analysis STA 409, Netzsch). Surface are l8 are determined by nitrogen adsorption using a standard volumetric BET apparatus. The tin(IV)oxide content of the loaded crtrriers and the catalysts is quantified gravimetrically. The platinum content of the catalysts is obtained by a spectrophotometric method which has been described elsewhere (11). 

Thermal Decomposition of Polymeric Nanocomposites Based on Anionic Clays The thermal decomposition of DGEBA nanocomposites cured with polyoxypropylene diamine (Jeffamine D230) and containing 4-toluenesul-fonate/LDH was investigated by simultaneous thermal analysis (STA) in air. The LDH nanocomposite (TS/LDH) is compared to the neat epoxy and to a bis(2-hydroxyethyl)ammonium montmorillonite nanocomposite (30B). The clay content was 5 wt% for both nanocomposites. In Figure 9.24, differential thermal analyses obtained by STA are shown. A main exothermic peak is observed at about 550° C for neat epoxy. In the LDH nanocomposite this peak is split in two parts, so the heat release rate is decreased and the heat evolution delayed, where as no relevant difference is observed between neat epoxy and the cationic clay nanocomposite. 

Simultaneous thermal analysis (STA) refers to the simultaneous application of two or more thermoan-alytical methods on one sample at the same time, such as DTA and thermoconductivity. In practice, however, this term is mostly used for simultaneous measurement of the mass changes and caloric effects on a sample under thermal treatment. The benefits are (i) information on transformation energetics and mass change in one run, under identical conditions (ii) time saving and (Hi) no differences in sample composition for the various thermal measurements - important for non-homogeneous sample materials. Although TG-DSC and TG-DTA are the most widely used of the simultaneous techniques due to... 

Two different thermal methods were used for the analysis of the high-temperature behavior of the various ash san5>Ies, i.e., simultaneous DTA/TGA using a NETSCH STA 429 friermal analysis instrument, and sintering tests performed in a simple muffle furnace, both in combination with a SEM/EDX technique for the elemental analysis of the thermally treated ash samples, using a JEOL 6300 scaiming microscope. 

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