Thermal sampling method

Poling and heating profiles used to measure thermally stimulated current. (1) Standard measurement, (11) partial heating method or peak cleaning method (111) thermal sampling method... 

Figure 2.26 Temperature and applied field diagram for the thermal sampling method...

A reliable determination of the adsorbent temperature is obviously a crucial requirement of the thermal desorption method. Thermocouples are mostly used to this end. With disks and foils, a thermocouple can be spot-welded onto the back or edge of the sample. Thermocouples can be attached also to ribbons as well as to the wall of the vessel containing an evaporated film. With powdered adsorbents, thermocouples are located in the layer of the sample. The adsorbents in the form of filaments and ribbons are frequently used simultaneously as resistance thermometers, switched... 

In contrast to thermal ionization methods, where the tracer added must be of the same element as the analyte, tracers of different elemental composition but similar ionization efficiency can be utilized for inductively coupled plasma mass spectrometry (ICPMS) analysis. Hence, for ICPMS work, uranium can be added to thorium or radium samples as a way of correcting for instrumental mass bias (e g., Luo et al. 1997 Stirling et al. 2001 Pietruszka et al. 2002). The only drawback of this approach is that small inter-element (e g., U vs. Th) biases may be present during ionization or detection that need to be considered and evaluated (e.g., Pietruszka et al. 2002). 

The use of conventional photographic systems for data acquisition, printing and archiving results of planar chromatography [401] has now largely been superseded by video documentation systems. A sample method for documentation of TLC plates has been described by a combination of computer, scanner, and digital colour thermal printer resulting in a very... 

The most common precolumn chromatographic techniques discussed here are SFE (Section 3.4.2), SPE (Section 3.5.1) and SPME (Section 3.5.2). However, sampling methods such as thermal desorption, pyrolysis and headspace (Section 4.2.2) may also be classified in this category. 

Applications The potential of a variety of direct solid sampling methods for in-polymer additive analysis by GC has been reviewed and critically evaluated, in particular, static and dynamic headspace, solid-phase microextraction and thermal desorption [33]. It has been reported that many more products were identified after SPME-GC-MS than after DHS-GC-MS [35], Off-line use of an amino SPE cartridge for sample cleanup and enrichment, followed by TLC, has allowed detection of 11 synthetic colours in beverage products at sub-ppm level [36], SFE-TLC was also used for the analysis of a vitamin oil mixture [16]. 

SFE-GC-MS is particularly useful for (semi)volatile analysis of thermo-labile compounds, which degrade at the higher temperatures used for HS-GC-MS. Vreuls et al. [303] have reported in-vial liquid-liquid extraction with subsequent large-volume on-column injection into GC-MS for the determination of organics in water samples. Automated in-vial LLE-GC-MS requires no sample preparation steps such as filtration or solvent evaporation. On-line SPE-GC-MS has been reported [304], Smart et al. [305] used thermal extraction-gas chromatography-ion trap mass spectrometry (TE-GC-MS) for direct analysis of TLC spots. Scraped-off material was gradually heated, and the analytes were thermally extracted. This thermal desorption method is milder than laser desorption, and allows analysis without extensive decomposition. 

The structure of the catalysts was characterized by X-ray diffraction, IR-spectroscopy and transmission electron microscopy, their thermal stability was followed by thermal analytical method. The specific surface area and pore size distribution of the samples were determined by nitrogen adsorption isotherms. 

The thermal resistance between the ends of the sample and the copper blocks must be negligible compared with the thermal resistance of the sample. This assumption must be verified especially for short samples at low temperature where the contact resistance is higher. For this reason, a second measurement of the thermal conductivity of Torlon in the 4.2-25 K range was carried out. The second sample had a different length (L = 24.51 mm) and the same section A. This additional measurement gave the same value of k within 2%. Moreover, we see from Fig. 11.15 that data of thermal conductivity at 4.2 K well join data at lower temperatures (within 3%) obtained on a sample of much smaller geometrical factor and with a different method (integrated thermal conductivity method) and a different apparatus [38], Finally, at room temperature, we find k = 0.26 W/mK, which is the data sheet value. 

The sample temperature is increased in a linear fashion, while the property in question is evaluated on a continuous basis. These methods are used to characterize compound purity, polymorphism, solvation, degradation, and excipient compatibility [41], Thermal analysis methods are normally used to monitor endothermic processes (melting, boiling, sublimation, vaporization, desolvation, solid-solid phase transitions, and chemical degradation) as well as exothermic processes (crystallization and oxidative decomposition). Thermal methods can be extremely useful in preformulation studies, since the carefully planned studies can be used to indicate the existence of possible drug-excipient interactions in a prototype formulation [7]. 

A reliable procedure for determination of molecular parameters number, weight and z-averages of the molecular weight (Mj, i = n, w and z respectively) for polyethylenes, PE, by means of Size Exclusion Chromatography, SEC, has been developed. The Waters Sci. Ltd. GPC/LC Model 150C was used at 135 C with trichlorobenzene, TCB, as a solvent. The standard samples as well as commercial stabilized and not stabilized PE-resins were evaluated. The effects of sampling, method of solution preparation, addition of antioxidant(s), thermal and shear degradation were studied. The adopted procedure allows reproducible determination of and M , with a random error of 4% and M2, with 9%, within 2 to 72 hrs from the initial moment of preparation of solutions. 

M P kBT/H) for the a- and Iz-directions and kc = MP(kBT/K) for the c-direction of the classical dipole. The same sampling method from the CMC simulations can be applied to the classical system NP dipoles with the potential energy from Eq. 13 to obtain thermally averaged values of quantities of interest. Thus, thermally averaged value ( Sc I > of the quantum system is given by ... 

Modified filter sampling methods that are available will measure ambient levels of strong acid in ambient aerosol samples, and these methods do so with acceptable precision and accuracy [as indicated by the balance between measured anions and cations (56, 57)] in the absence of significant levels of particulate weak acids. Additional intercomparisons involving intrinsically different techniques for particulate strong acidity [e.g., IR spectroscopy (48), thermal speciation (38, 45), and filter methods (28)] are needed. Further information on the occurrence of various weak acids in airborne particles is needed, along with further studies of techniques for their specific determination in atmospheric aerosol samples. 

Thermally stimulated methods are based on the fact that a sample frozen in a deformed or polarized state gradually returns to equilibrium as various types of molecular motions set in with increasing temperature. 

Notes The most commonly used porous polymer sorbent is Tenax-GC, although the Porapakand Chromosorb Century series have also been used Tenax-GC has been used with thermal desorption methods, but can release toluene, benzene, and trichloroethylene residues at higher temperatures in addition to Tenax-GC, XAD 2-8, Porapak-N, and Chromosorbs 101, 102, 103, and 106 have found applications, sometimes in stacked sampling devices (for example, a sorbent column of Tenax-GC — Chromosorb 106 in tandem) Chromosorb 106, a very low polarity polymer, has the lowest retention of water with respect to organic materials and is well suited for use as a backup sorbent... 

It has been shown that in some polymers the effect of e+ exposure on I3 is completely reversible if the samples are annealed at temperatures near or above their Tg s. This implies that in thermal studies, methods should be developed... 

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