Micro-furnace pyrolysis

Another very flexible solution for numerous applications in pyrolysis, outgassing or thermal extraction experiments is the use of a micro-furnace, which can be resistively heated to temperatures above 1000 C (Roussis and Fedora, 1998). The sample is placed in a small, low, thermal mass cup of 50-80 pL volume, which is dropped into the heated pyrolysis furnace consisting of a vertical quartz tube. The furnace tube size is comparable to a GC inlet liner with 4.5 mm inner diameter and 12 mm length and allows programmable temperature profiles with heating rates of up to 200 C/min (Frontier Laboratories Ltd., Japan). 

Typical sample sizes are in the 0.1 mg range, allowing a fast heat transfer to the set desorption or pyrolysis temperature. The transfer of the pyrolysis products is achieved by a carrier gas flow through the heated zone and a needle tip on the bottom of the furnace reaching into the injector of the GC. 

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Figure 239 Five micro-furnace pyrolysis tubes for different pyrolysis and thermal desorption applications. (Frontier Laboratories Ltd., Japan.) (a) Liquid sampler for direct liquid sample injection using a micro syringe, (b) Single-shot sampler for flash pyrolysis using sample cup. (c) On-line micro reaction...

Figure 11.9 Pyrogram of a paint sample collected from sixteenth century wall paintings in the Messer Filippo cell of the tower in Spilamberto, Italy. Pyrolysis was performed with a micro furnace pyrolyser, at 600°C, in the presence of HMDS. 1, Carbohydrate pyrolysis products 2, lauric acid 3, suberic acid 4, levoglucosane 5, azelaic acid 6, miristic acid 7, hexadecanenitrile 8, palmitic acid 9, octadecanenitrile 10, oleic acid 11, stearic acid. TMS derivative [74]...

FIGURE 8.1 Pyrolysis unit, Scientific Glass Engineering (SGE) Pyrojector. 1. Sample loading area, 2. Quartz sample tube (reaction zone), 3. Sample loading cover interlock, 4. Valve body, 5. O-ring type seal, 6. Carrier gas inlet, 7. Check valve, 8. Carrier gas vent, 9. Valve spindle, 10. Heat deflectors, 11. Micro furnace,... 

Micro)furnace pyrolysers, which are preheated to the desired final pyrolysis temperature before introduction of the sample, are categorised as continuousmode pyrolysers. In such devices, the sample is either moved into a preheated pyrolysis chamber (isothermal mode) or heated rapidly from ambient to pyrolysis temperature (programmable mode). However, furnace pyrolysers are generally held isother-maUy at the desired pyrolysis temperature, and the samples are introduced into the hot volume. 

Figures 2.1 and 2.2 illustrate the schematic flow diagrams of the measuring systems of the pyrolysis (Py)-GC/MS and evolved gas analysis (EGA)—MS, respectively. In both systems, the vertical micro-furnace pyrolyzer (Frontier Lab., PY-2020iD) mounted on...

Besides the flash pyrolysis of solid samples, the furnace solution allows different sampling devices for a wider bandwidth of analytical experiments (see Figure 2.39). This solution can provide access to additional analytical applications with the introduction of liquid samples using a regular micro syringe, the online pyrolysis for the analysis of high-pressure reactions in glass capsules, the thermal desorption of small amounts of solid materials, or the combination with a subsequent second reactor for the reaction with catalyst materials. Unique is the... 

Spray pyrolysis (SP) has been used to produce micro-and nanosized particles since the 1990s [50]. In a typical SP synthesis of Cu NPs, an aqueous solution of the correct precursor is atomized and the resultant droplets are transferred by a carrier gas into a tubular furnace (a possible instrumental set-up is shown in Figure 1.3), where the precursor is converted into spherical Cu NPs (see Figure 1.4) [51]. The... 

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