Atmospheric pressure thermal desorption

Paglia G, D Apolito O, Corso G. Precursor ion scan profiles of acylcarnitines by atmospheric pressure thermal desorption chemical ionization tandem mass spectrometry. Rapid Commun Mass Spectrom 2008 22 3809-3815. 

El = electron ionization Cl = chemical ionization ES = electrospray APCI = atmospheric-pressure chemical ionization MALDI = matrix-assisted laser desorption ionization PT = plasma torch (isotope ratios) TI = thermal (surface) ionization (isotope ratios). 

Electrospray ionization [21] is one of the most widely utilized ionization techniques employed today for the analysis of thermally fragile molecules. As such, it has assumed an important role in the analysis of biologically important molecules. ESI is a desorption ionization technique. This means that ions are formed before or during the transition from the liquid phase and need not be volatilized in advance of the ionization event (as is the case for El, Cl, etc.). Like APCI and APPI, ESI occurs at atmospheric pressure outside the vacuum chamber of the mass spectrometer (Fig. 11.5). A solution of the analyte passes through... 

Today s coke plant gas purification processes are mostly carried out under atmospheric pressure, employing a circulated ammonia-based absorbent. The consumption of the external solvent is reduced via the use of ammonia available in the coke gas (138). An example of innovative purification processes is the ammonia hydrogen sulfide circulation scrubbing (ASCS) (Figure 17), in which the ammonia contained in the raw gas dissolves in the NH3 absorber and then the absorbent saturated with the ammonia passes through the H2S absorber to selectively absorb the H2S and HCN components from the coke gas. The next step is the thermal regeneration of the absorbent with the steam in a two-step desorption plant, whereas a part of the deaciditied water is fed back into the H2S absorber (25). 

In the first thermal desorption experiments under ambient pressure and in a hydrogen atmosphere up to 1 MPa several endothermic peaks were observed... 

Flow adsorption microcalorimetry has been used to measure the heats of adsorption of ammonia in a nitrogen carrier on the H and Na forms of a Y zeolite [21]. The calorimeter was linked to a thermal conductivity detector in which the rates of adsorption and desorption and the associated rates of heat evolution or absorption were measured simultaneously at atmospheric pressure. The authors found that, as surface coverage increased, the sites covered first were not necessarily those with the highest molar heats of adsorption. 

To perform mass spectrometry, one must make ions from neutral molecules. Ionization methods have advanced from the classic electron ionization (El), through chemical ionization, field desorption, fast atom bombardment (FAB), h 62 thermospray to the atmospheric pressure ionization (API) techniques currently favored. El is classic, but its is restricted to thermally stable, volatilizable compounds. Field desorption was always a specialized niche technique applicable to some larger compounds. Fast atom bombardment enjoyed a meteoric rise in use when it was first reported in 1981 but it has all but disappeared now, being replaced by the API tech-... 

Wu, J. et al., High-throughput cytochrome P450 inhibition assays using laser diode thermal desorption-atmospheric pressure chemical ionization-tandem mass spectrometry, Anal. Chem., 79, 4657, 2007. 

Nitrogen capacities for pure gas were determined In a similar manner. Following activation, the adsorbent beds were allowed to equilibrate 1n a stream of dry nitrogen at 30°C. Thermal desorption coupled with void volume measurements by helium displacement into a gas buret at atmospheric pressure yielded the amount of nitrogen adsorbed. 

In a series of papers, Suvorov et al. investigated heterogeneous catalysis of the cyclization of isolated aldehyde and ketone phenylhydrazones. y-Alumina was typically employed as catalyst in the vapor phase reaction at atmospheric pressure and at temperatures around 300 °C. A maximum yield of 60% was obtained from acetaldehyde phenylhydrazone as a result of thermal decomposition of the hydrazone [7] and the formation of benzene and aniline as by-products [8]. Kinetic studies indicated that the rate-determining step was desorption of product from the surface [9]. 

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