Thermal analysis simultaneous analyzers

The thermal properties of benzoic acid were evaluated using simultaneous differential thermal analysis (DTA) and thermogravimetric analysis (TGA). This work was performed on a Shimadzu DT-30 Thermal Analyzer system, which was calibrated using indium standard. Using a heating rate of 10°C/min, the thermograms presented in Figure 3 were obtained. 

To obtain the cure kinetic parameters K, m, and n, cure rate and cure state must be measured simultaneously. This is most commonly accomplished by thermal analysis techniques such as DSC. In isothermal DSC testing several different isothermal cures are analyzed to develop the temperature dependence of the kinetic parameters. With the temperature dependence of the kinetic parameters known, the degree of cure can be predicted for any temperature history by integration of Equation 8.5. 

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). 

Thermal gravimetric analysis and differential thermal analysis (TGA/DTA) can be performed by using a SDT 2960 Simultaneous Differential Thermal Analyzer (TA Instruments, Inc., New Castle, DE). The instrument was calibrated with gold supplied by Perkin-Ehner. Samples (70 mg) of as-prepared powders were hand-pressed in a 3 mm dual action die and placed inside Pt sample cups and heated at the rates of 10 K/ min from ambient temperature to 1400°C. The reference material was used as a pellet of a-alumina. A flow of synthetic air at 50mL/min was maintained during the experiments. 

The reaction processes of substances cannot be analyzed by simple DTA/DSC or TG when thermal transition and the mass change due to reaction overlap. If DTA/DSC or TG is coupled with an evolved gas detector (EGD) and/or evolved gas analyzer (EGA), the reaction process can clearly be detected. Among various thermal analysis coupled simultaneous techniques [56], DTA/DSC or TG coupled with EGD and/or EGA is extensively used. TA-EGD-EGA coupled... 

The synthesis of 1,2, and 3 have been reported previously. All reactions were carried out in an inert atmosphere unless otherwise noted. Solvents were purified by established procedures. 1,3-Dichlorotetramethyldisiloxane and 1,5-dichlorohexamethyltrisiloxane were obtained from Silar Laboratories and used as received. -Butyllithium (2.5 M in hexane) was obtained from Aldrich and used as received. l,7-Bis(chlorotetra-methyldisiloxyl)-/w-carborane 1 was purchased from Dexsil Corporation. Hexachlorobutadiene was obtained from Aldrich and distilled before use. Cure and thermal analysis studies were performed on various mixtures of 1 and 3a in milligram quantities. Thermogravimetric analyses (TGA) were performed on a DuPont SDT 2960 Simultaneous DTA-TGA analyzer. Differential scanning calorimetry analyses (DSC) were performed on a DuPont 910 instrument. Unless otherwise noted, all thermal experiments were carried out at a heating rate of 10 °C/min and a nitrogen flow rate of 50 cc/min. 

Thermogravimetric and differential thermal analysis were also performed in a TA SDT 2%0 TG-DSC simultaneous instrument. Pt crucibles containing 5-7 mg of sample were heated at 2°C/min from room temperature to 1000 °C under dry oxidizing atmosphere. In order to verify the effectiveness of the separation method, several fractions during extraction process have been analyzed by above described techniques. 

The thermal studies were carried out on a Stanton Redcroft STA-780, simultaneous thermal analyzer series designed to give simultaneous differential thermal analysis (DTA) and differential thermogravimetry (DTG). 

The HREELS, Auger electron spectroscopy (AES) and thermal desorption spectrometry (TDS) experiments were carried out in a UHV chamber described previously.6 Briefly, the chamber was equipped with a HREELS spectrometer for vibrational analysis, a single-pass cylindrical mirror analyzer for AES measurements and a quadrupole mass spectrometer for TDS measurements. The HREELS spectra were collected in the specular direction with an incident energy of 3.5 eV and with a spectroscopic resolution of 50-80 cm-1. The TDS data were obtained by simultaneously monitoring up to 16 masses, with a typical heating rate of about 1.5 K s-1. 

Sample analysis by thermal ionization mass spectrometry (TIMS) results in measurement of isotopic ratios of minerals. Total mineral content of samples is then determined by one of two methods. One approach is to use flame atomic absorption spectrophotometry (AAS) to determine total mineral content of samples. Since AAS does not have the same level of precision as TIMS a sufficient number of replicates is analyzed for a mineral content determination with a CV of within 1%. Alternatively if a mineral has 3 or more isotopes and fractionation corrections are not made the following procedure may be used. An individual is fed one isotope and another isotope is added to the sample prior to analysis to determine the total mineral content of the sample by dilution of the second isotope. In this way both the amount of the isotope fed which is recovered in the feces and the total mineral content of the sample can be determined simultaneously. If fractionation corrections are to be made a mineral must have at least four isotopes. Details of these procedures will be reported separately. 

Simultaneously developing flow in annular sector ducts for air (Pr = 0.7) has been analyzed by Renzoni and Prakash [287]. In their analysis, the outer curved wall is treated as adiabatic, and the boundary condition is imposed on the inner curved wall as well as on the two straight walls of the sector. The fully developed friction factors, incremental pressure drop numbers, hydrodynamic entrance lengths, and thermal entrance lengths are presented in Table 5.62. The term L y used in Table 5.62 is defined as the dimensionless axial distance at which /app Re = 1.05/ Re. The fully developed Nusselt numbers are represented by Nu/< in order not to confuse the reader since the thermal boundary condition applied in Renzoni and Prakash [287] is different from those defined in the section. 

Shepherd Chenery (1995) pioneered the laser ablation ICP-MS (inductively coupled plasma-mass spectrometry) method of analyzing individual fluid inclusions. An UV laser ablation microprobe is used to drill a hole into a mineral, to reach an inclusion up to 60/zm below the sample surface. For the laser ablation procedure the sample is placed in a modified thermal vacuum cell. The elevated temperature in the ablation cell raises the internal vapor pressure of the inclusion, which causes instantaneous rupture and highly efficient fluid expulsion as the beam breaches the inclusion wall. The vacuum pulls the vaporized fluid into the ICP-MS, where it is analyzed for major and minor ion concentrations. The advantages of the ICP-MS method are the small spot size of the laser (<2 m), allows analysis of small inclusions (> 10/zm) in a variety of minerals (halite, calcite, quartz, and others). A wide range of ions can be analyzed simultaneously, including low concentrations of minor ions. With multicollector ICP-MS, it will be possible to analyze strontium isotopes and other stable isotopes (5 C, S 0, S S) in fluid inclusions. Laser ablation ICP-MS is not as precise as other methods ( 30%) and the results can only be reported as ionic ratios as the volume of an inclusion cannot be determined prior to analysis. However, if the concentration... 

One model of the above-mentioned Derivatograph (Hungarian Optical Works, Budapest) is designed for collecting and analyzing the decomposition products with the advantage of simultaneous monitoring of the TG, DTG and DTA curves (the technique is named thermal volatilization analysis TVA). 

---