Sample heat transfer

Probe The probe is constrncted of stainless steel and has Swagelok fittings top and bottom for attachment to the process sample line. The constrnction of the probe inclndes a Dewar that reduces the sample heat transfer throngh the walls of the probe to the magnet components. At the sampling zone the inner wall of the probe is constrncted of alnmina ceramic which is specialty welded to the stainless. The probe is pressure tested to 1.035 x 10" Pa (103.4 bar, 1500 psi). The duplexor and preamplifier are built into the base of the probe. 

Figure 6.28. Furnace and sample chamber. A. glass capillary tube for sample B. sample-holder plate C. sample heat transfer sleeve D. sample thermocouple E. furnace block G. reference capillary tube H. reference heat transfer sleeve J, reference thermocouple K, heater cartridge.

Carbonates decompose at relatively high temperatures, 660 to 740°C (1,220 to 1,364°F) for CaCO,3. When large samples are used the rate of decomposition can be controlled by the rate of heat transfer or the rate of CO9 removal. 

Apparatus for testing materials for heat-transfer applications is shown in Fig. 28-4. Here the sample is at a higher temperature than the bulk solution. 

That such a process is today commercially important is a measure of the success of chemical engineers in overcoming heat transfer problems involved with masses incapable of being stirred. An idea of the extent of the problem can be gauged from the fact that it takes six hours to cool a sample of polystyrene from 160°C using a cooling medium at 15°c when the heat transfer distance is two inches. 

In the case of a temperature probe, the capacity is a heat capacity C == me, where m is the mass and c the material heat capacity, and the resistance is a thermal resistance R = l/(hA), where h is the heat transfer coefficient and A is the sensor surface area. Thus the time constant of a temperature probe is T = mc/ hA). Note that the time constant depends not only on the probe, but also on the environment in which the probe is located. According to the same principle, the time constant, for example, of the flow cell of a gas analyzer is r = Vwhere V is the volume of the cell and the sample flow rate. 

Figure 6.8 Schematic diagram of a typical interface used for on-line SFE-SFC coupling (from ref. 42) 1, pump 2, heated transfer line 3, valve 4, sample concentrator 5, valve 6, SFC unit.

How frequently the oil condition should be tested depends on operating and atmospheric conditions after the commissioning sample, further samples should be taken at three months and one year after the unit is first energized. After this, under normal conditions, testing should be carried out annually. In unfavorable operating conditions (damp or dust-laden atmospheres, or where space limitations reduce air circulation and heat transfer) testing should be carried out every six months. 

Where large samples of reactant are used and/or where C02 withdrawal is not rapid or complete, the rates of calcite decomposition can be controlled by the rate of heat transfer [748] or C02 removal [749], Draper [748] has shown that the shapes of a—time curves can be altered by varying the reactant geometry and supply of heat to the reactant mass. Under the conditions used, heat flow, rather than product escape, was identified as rate-limiting. Using large ( 100 g) samples, Hills [749] concluded that the reaction rate was controlled by both the diffusion of heat to the interface and C02 from it. The proposed models were consistent with independently measured values of the transport parameters [750—752] whether these results are transfenable to small samples is questionable. 

FIGURE 6.12 A bomb calorimeter is used to measure heat transfers at constant volume. The sample in the central rigid container called the bomb is ignited electrically with a fuse wire. Once combustion has begun, energy released as heat spreads through the walls of the bomb into the water. The heat released is proportional to the temperature change of the entire assembly. 

The heat transfer and pressure drop in a rectangular channel with sintered porous inserts, made of stainless steels of different porosity, were investigated. The experimental set-up is shown in Fig. 2.9. Heat fluxes up to 6MW/m were removed by using samples with a porosity of 32% and an average pore diameter of 20 pm. Under these experimental conditions, the temperature difference between the wall and the bulk water did not exceed AT = 55 K at a pressure drop of AP = 4.5 bars (Hetsroni et al. 2006a). 

Fig. 1 shows the thermal decomposition curves of HDPE mixed with Al-MCM-41, with respect to time, at isothermal operating temperatures. Lag periods were formed at the initial stage of decomposition, possibly due to the heat transfer effect, which could delay the decomposition of a sample until the latter reaches the operating temperatures. As the reaction ten erature increased, the reaction time became noticeably shorter. The shortening of the reaction time was clearly observed when the reaction occurred at the reaction teirperatures between 420 and 460 °C. The HDPE on Al-MCM-41-P decomposed faster than that on blank and that on A1-MCM-41-D, as shown in Fig. 1(b). 

Four mmoles of malononitrile and benzaldehyde were introduced in a batch stirred tank reactor at 323 K with toluene as solvent (30 ml). Then 0.05 g of aluminophosphate oxynitride was added. Samples were analysed by gas chromatography (Intersmat Delsi DI200) using a capillary column (CPSilSCB-25 m). Care was taken to avoid mass or heat transfer limitations. Before the reaction no specific catalyst pretreatment was done. 

The catalytic experiments were performed at the stationnary state and at atmospheric pressure, in a gas flow microreactor. The gas composition (NO, CO, O2, C3H, CO2 and H2O diluted with He) is representative of the composition of exhaust gases. The analysis, performed by gas chromatography (TCD detector for CO2, N2O, O2, N2, CO and flame ionisation detector for C3H6) and by on line IR spectrometry (NO and NO2) has been previously described (1). A small amount of the sample (10 mg diluted with 40 mg of inactive a AI2O3 ) was used in order to prevent mass and heat transfer limitations, at least at low conversion. The hourly space velocity varied between 120 000 and 220 000 h T The reaction was studied at increasing and decreasing temperatures (2 K/min) between 423 and 773 K. The redox character of the feedstream is defined by the number "s" equal to 2[02]+[N0] / [C0]+9[C3H6]. ... 

HREELS experiments [66] were performed in a UHV chamber. The chamber was pre-evacuated by polyphenylether-oil diffusion pump the base pressure reached 2 x 10 Torr. The HREELS spectrometer consisted of a double-pass electrostatic cylindrical-deflector-type monochromator and the same type of analyzer. The energy resolution of the spectrometer is 4-6 meV (32-48 cm ). A sample was transferred from the ICP growth chamber to the HREELS chamber in the atmosphere. It was clipped by a small tantalum plate, which was suspended by tantalum wires. The sample was radia-tively heated in vacuum by a tungsten filament placed at the rear. The sample temperature was measured by an infrared (A = 2.0 yum) optical pyrometer. All HREELS measurements were taken at room temperature. The electron incident and detection angles were each 72° to the surface normal. The primary electron energy was 15 eV. 

Figure 8.26(A) is an example of a valve type interface [329]. Helium carrier gas is provided to the headspace saiq)ler and is split into two flow paths. One path is flow-controlled and provides a constant flow of carrier gas which passes from the headspace unit through the heated transfer line to the gas chromatograph. The second flow path is pressure-regulated and, in the standby mode, the seunple loop and seuapling needle are flushed continuously by the helium flow. At a time determined by the operator, the sampling needle pierces the septum and helium pressurizes the headspace vial to any desired pressure. The headspace gas is then allowed to vent through the sample loop. Once filled, the sample loop is placed in series with the normal carrier gas flow and its contents are driv Bbhrough the heated...

The geometry of the tubes allows the heat transfer being considered one dimensional, and each tube to be a lumped system in front of the ambient air. This two conditions are fulfilled when Bi < 0.1 (Biot number Bi = a /(/(2a ), where R is the radius of the sample, X its thermal conductivity and a the heat transfer coefficient between the tube and the environment). Once the temperature-time curves of the PCM and the reference substance are obtained (Figure 160), the data can be used to determine the thermophysical properties of the PCM. 

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